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Preparation method of zeolite molecular sieve monolith with composite pore structure

A zeolite molecular sieve and composite pore technology, which is applied in molecular sieve catalysts, crystalline aluminosilicate zeolites, chemical instruments and methods, etc., can solve the difficulties in the preparation of composite pore structure zeolite materials and the amorphous pore walls of mesoporous materials, etc., to achieve Effects of reducing induction time, improving stability, and lowering reaction temperature

Active Publication Date: 2010-09-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 2. Transcrystallization of amorphous pore walls in mesoporous materials
[0007] It can be seen from the above that although researchers from various countries have developed many synthetic methods, the preparation of composite pore structure zeolite materials is still one of the difficulties in the field of synthesis.

Method used

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  • Preparation method of zeolite molecular sieve monolith with composite pore structure
  • Preparation method of zeolite molecular sieve monolith with composite pore structure
  • Preparation method of zeolite molecular sieve monolith with composite pore structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] a) Mix polyethylene glycol, 0.4 mol / liter nitric acid solution and aluminum nitrate, dissolve it and transfer it to an ice-water mixing bath, add tetraethyl orthosilicate, stir for 2 hours, transfer it to a mold and seal it, and react at 60°C 24 hours. Sample A was obtained after demoulding and drying. Among them, the mass ratio of polyethylene glycol / SiO 2 =0.35,H + / SiO 2 =0.16,H 2 O / SiO 2 =2.25, Al 2 o 3 / SiO 2 = 0.004.

[0028]b) Sample A was impregnated dropwise with 0.84 mol / L sulfuric acid solution overnight, dried in sections at 60°C and 170°C, and then roasted at 800°C under nitrogen protection to obtain Sample B. Among them, the mass ratio of sulfuric acid / SiO 2 = 0.1.

[0029] c) Place the sample B in the porous support on the upper layer of the reaction kettle, place a tetraethylammonium hydroxide solution with a volume ratio of 8 to the sample B, and crystallize at 160°C for 6 days.

[0030] After leaving the kettle, the product was washed with ...

Embodiment 2

[0032] a) Mix citric acid, polyoxyethylene-polyoxypropylene-polyoxyethylene, and 1 mol / liter acetic acid solution, dissolve and transfer to an ice-water mixing bath, add tetramethyl orthosilicate, and stir vigorously for 0.1 hour Transfer to a mold to seal, and react at 40°C for 48 hours. After taking it out, it was demolded and dried to obtain sample A. Among them, the mass ratio of citric acid / SiO 2 =0.5, polyoxyethylene-polyoxypropylene-polyoxyethylene / SiO 2 =0.3,H + / SiO 2 =0.25,H 2 O / SiO 2 = 2.5.

[0033] b) Sample A was impregnated overnight in 18.4 mol / L sulfuric acid solution, dried in sections at 120°C and 200°C, and then roasted at 700°C under nitrogen protection to obtain sample B. Among them, the mass ratio of sulfuric acid / SiO 2 = 0.15.

[0034] c) Add sample B to a mixed solution of sodium hydroxide, tetrapropylammonium bromide, aluminum isopropoxide and water, soak it overnight and transfer it to the porous bracket on the upper layer of the reaction ket...

Embodiment 3

[0037] a) Mix polyoxyethylene-polyoxypropylene-polyoxyethylene, 1 mol / liter hydrochloric acid solution and aluminum chloride, add tetrapropyl orthosilicate after dissolving, stir at 40°C for 5 hours, transfer to a mold and seal, Sample A was obtained by reacting at 80° C. for 24 hours. Among them, the mass ratio of polyoxyethylene-polyoxypropylene-polyoxyethylene / SiO 2 = 1.0, H + / SiO 2 =0.2,H 2 O / SiO 2 = 4, Al 2 o 3 / SiO 2 = 0.4.

[0038] b) Remove the sample A and then dry it. Add a mixed solution of sucrose, concentrated sulfuric acid and deionized water, soak overnight at 100°C and 180°C in stages, and bake at 900°C under nitrogen protection to obtain sample B. Among them, the mass ratio of sucrose / SiO 2 =1, sulfuric acid / SiO 2 =0.1, water / SiO 2 =2.

[0039] c) Place the sample B in the porous support on the upper layer of the reaction kettle, place a tetraethylammonium hydroxide solution with a volume ratio of 10 to the sample B, and crystallize at 180° C. fo...

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Abstract

The invention relates to a preparation method of a zeolite molecular sieve monolith with a composite pore structure, which mainly solves the problem that a composite-pore molecular sieve which has both mesopores (or macropores) and a zeolite pore wall is difficult to obtain in the prior art. The zeolite molecular sieve monolith with bicontinuous macropores and three-dimensional communicated mesoporous paths is prepared from a macroporous silicagel monolith used as a substrate by using a method of in-situ carbonizing protection or secondary carbon addition by using carbon sources and then vapor-phase crystallization. The molecular sieve with excellent diffusivity has important application prospect in fields of catalysis, absorption, separation and the like.

Description

technical field [0001] The invention relates to a preparation method of zeolite molecular sieve monolith with composite pore structure. Background technique [0002] Zeolite molecular sieve materials have the advantages of regular microporous structure, high hydrothermal stability, and suitable surface acidity and alkalinity, so they have become one of the most commonly used catalysts in petrochemical processes. However, with the continuous development of science and technology and the continuous improvement of the requirements of the petroleum industry for raw materials to be "dried and squeezed out", traditional zeolite molecular sieves gradually show their shortcomings. This is mainly due to the fact that zeolite molecular sieves only have a microporous structure, which greatly limits the mass transfer and diffusion of macromolecules such as heavy oil components in the catalyst, thereby inhibiting the reactivity, selectivity and life of the catalyst. [0003] In order to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04B01J29/06B01J29/40
Inventor 刘茜谢在库杨贺勤李宏旭高焕新
Owner CHINA PETROLEUM & CHEM CORP
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