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A kind of synthetic method of nano zsm-5 molecular sieve aggregate

A technology of ZSM-5 and synthetic method, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of low recovery rate of fine particles, unconventional, complicated separation and treatment process, etc. Achieve the effect of reducing operation and processing costs, reducing processing costs, and simplifying the process

Active Publication Date: 2020-11-06
WISON ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In view of the above-mentioned shortcoming of the prior art, the object of the present invention is to provide a kind of synthetic method of nanometer ZSM-5 molecular sieve aggregate, for solving one of problems in the prior art is prior art synthetic nanometer ZSM-5 molecular sieve needs The use of expensive or unconventional templating agents that are not easy to obtain in large quantities, or the need to introduce a large amount of dispersants (electrolytes or surfactants) into the system leads to complex synthesis, separation and treatment processes and high costs. The second problem is high dispersion. ZSM-5 molecular sieve with nano-fine particles cannot be separated by conventional means and the recovery rate of fine particles is low

Method used

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  • A kind of synthetic method of nano zsm-5 molecular sieve aggregate
  • A kind of synthetic method of nano zsm-5 molecular sieve aggregate
  • A kind of synthetic method of nano zsm-5 molecular sieve aggregate

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Effect test

Embodiment 1

[0046] 1) mixing the acidified aluminum source solution and the alkaline silicon source solution to obtain the mother liquor of the molecular sieve; the acidified aluminum source solution includes aluminum sulfate, water and sulfuric acid; the alkaline silicon source solution includes water glass (modulus 3.2 ~3.4), water, n-butylamine, and nano-aggregate all-silicon molecular sieve seed crystals that have only undergone low-temperature drying treatment, the particle size is no more than 200nm, and the morphology is an aggregated state formed by the accumulation of primary particles of 10-30nm; in the molecular sieve mother liquor , Na 2 O: Al 2 o 3 : SiO 2 :H 2 O: n-butylamine molar ratio is 0.20:0.04:1:50:0.32; 2 5% by weight;

[0047] 2) After the molecular sieve mother liquor was ultrasonically oscillated at 50kHz for 0.5 hours, the mixed solution was transferred to a 5L autoclave for hydrothermal stirring and crystallization. The hydrothermal crystallization was divi...

Embodiment 2

[0049] 1) mixing an acidified aluminum source solution and an alkaline silicon source solution to obtain a molecular sieve mother liquor; the acidified aluminum source solution includes aluminum nitrate, water and sulfuric acid; the alkaline silicon source solution includes solid sodium silicate powder, Water, ethylenediamine, and nano-aggregate all-silicon molecular sieve seed crystals that have only undergone low-temperature drying treatment, the particle size does not exceed 200nm, and the appearance is an aggregated state formed by the accumulation of primary particles of 10-30nm; in the molecular sieve mother liquor, Na 2 O: Al 2 o 3 : SiO 2 :H 2 The molar ratio of O: ethylenediamine is 0.18:0.04:1:50:0.32; nano-aggregate all-silicon molecular sieve seeds account for SiO 2 5% by weight;

[0050] 2) After the molecular sieve mother liquor was ultrasonically oscillated at 50kHz for 2.0 hours, the mixed solution was transferred to a 5L autoclave for hydrothermal stirring...

Embodiment 3

[0052] 1) mixing the acidified aluminum source solution and the alkaline silicon source solution to obtain the molecular sieve mother liquor; the acidified aluminum source solution includes aluminum chloride, water and hydrochloric acid; the alkaline silicon source solution includes water glass (modulus 3.2-3.4), water, n-propylamine, and nano-aggregate all-silicon molecular sieve seed crystals that have only been dried at low temperature. , Na 2 O: Al 2 o 3 : SiO 2 :H 2 O: n-propylamine molar ratio is 0.20:0.05:1:40:0.32; 2 7% by weight;

[0053] 2) After the molecular sieve mother liquor was ultrasonically oscillated at 50kHz for 5 hours, the mixed solution was transferred to a 5L autoclave for hydrothermal stirring and crystallization. The hydrothermal crystallization was divided into two stages, and the hydrothermal crystallization temperature of the first stage was The crystallization time at 100°C is 24 hours, and the hydrothermal crystallization temperature of the...

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Abstract

The invention provides a nanometer ZSM-5 molecular sieve aggregate synthesis method, which comprises: 1) mixing an acidified aluminum source solution and an alkaline silicon source solution to obtaina molecular sieve mother liquor, wherein the acidified aluminum source solution comprises an aluminum source, water and mineral acid, and the alkaline silicon source solution comprises a silicon source, water, small molecule organic amine and active seed crystal, or a silicon source, water, sodium hydroxide, small molecule organic amine and active seed crystal; and 2) carrying out ultrasonic vibration on the molecular sieve mother liquor to uniformly disperse, transferring to an autoclave, carrying out hydrothermal crystallization (in two stages), carrying out conventional filtration, washing,drying, and calcining to obtain a high-crystallinity nanometer ZSM-5 molecular sieve aggregate, wherein the primary particle size is 20-50 nm, and the secondary morphology is the micro-elliptical particle formed by agglomerating the primary nanoparticles. According to the present invention, the prepared ZSM-5 molecular sieve aggregate has the good catalytic performance of the nanometer molecularsieve, and further has the advantages of the micrometer particle molecular sieve in filtration separation and acid washing recovery.

Description

technical field [0001] The invention belongs to the field of aluminosilicate zeolite synthesis, and relates to a method for synthesizing nano ZSM-5 molecular sieve aggregates. Background technique [0002] Zeolite is a crystalline microporous aluminosilicate, which is composed of silicon-oxygen tetrahedron and aluminum-oxygen tetrahedron interconnected by covalent bonds. It has a large specific surface area, good hydrothermal stability, excellent ion exchange performance and rich physical and chemical properties on the surface. Tunable, it has a wide range of applications in catalysis, adsorption, ion exchange and functional materials, especially in the field of industrial catalysis. ZSM-5 zeolite molecular sieve (USP 3702886) has a unique three-dimensional pore structure and acid properties. As a superior catalytic material, it has been used in the type-selective catalytic cracking, isomerization, alkylation, disproportionation, dewaxing, ester It plays an irreplaceable ro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/40B82Y30/00
CPCB82Y30/00C01B39/40C01P2002/72C01P2004/03C01P2004/62
Inventor 卓佐西黄孟凯李猛杨文书
Owner WISON ENG
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