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Synthesis method of nanometer needle-like ZSM-11 and mixed-crystal molecular sieve thereof

A technology of ZSM-11 and synthesis method, which is applied in the field of molecular sieves, can solve the problem of long micropore diffusion path, achieve the effect of strong operation purpose, controllable technology and cost, and shorten the intracrystalline micropore diffusion path

Active Publication Date: 2020-01-03
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for synthesizing nanoacicular ZSM-11 and its mixed crystal molecular sieve, so as to solve the problem that the microporous diffusion path in the existing conventional morphology ZSM-11 molecular sieve crystal is too long in the background technology

Method used

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  • Synthesis method of nanometer needle-like ZSM-11 and mixed-crystal molecular sieve thereof

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Effect test

Embodiment 1

[0023] 1) Add 173g of distilled water, 2.05g of aluminum sulfate, 4.08g of aluminum isopropoxide, 5.6g of sulfuric acid, 12.7g of tetrapropylammonium hydroxide, 29g of tetrabutylammonium bromide, and 54g of dodecyltrimethylammonium bromide After being placed in the hydrothermal synthesis kettle, stir evenly; slowly add 19.3g of silica sol with a mass fraction of 30% drop by drop under stirring, stir evenly, then add 18g of sodium hydroxide, and then seal the synthesis kettle; at a temperature of 50°C And under the condition of stirring speed 120r / min, aging treatment was carried out to synthetic solution for 32 hours, then down to room temperature, and open the kettle lid;

[0024] 2) After adding 308g of methanol to the synthesis liquid after aging treatment, seal the synthesis tank, crystallize at a temperature of 160°C and a stirring rate of 500r / min for 120 hours, cool to room temperature, discharge, wash, and separate , dried and roasted to obtain acicular ZSM-11 molecula...

Embodiment 2

[0026] 1) Mix 21.6g distilled water, 0.06g pseudoboehmite, 0.02g sodium metaaluminate, 1.8g hydrochloric acid, 5.3g tetrapropylammonium bromide, 3.08g dodecyltrimethylammonium bromide, 3.36g After tetradecyltrimethylammonium bromide is added in the hydrothermal synthesis kettle, stir evenly; under stirring state, slowly add 37.4g of water glass with a mass fraction of 38% and 3g of silicon oxide powder, stir evenly, and then add 16g Potassium hydroxide, and then seal the synthesis kettle; under the condition that the temperature is 12°C and the stirring rate is 900r / min, the synthesis liquid is aged for 149 hours, cooled to room temperature, and the lid of the kettle is opened;

[0027] 2) After adding 115g of ethanol and 75g of formaldehyde to the synthesis liquid after aging treatment, seal the synthesis kettle, crystallize at a temperature of 100°C and a stirring rate of 900r / min for 300 hours, cool to room temperature, discharge, Washing, separating, drying and calcining t...

Embodiment 3

[0029] 1) 1440g distilled water, 0.125 aluminum nitrate, 32g nitric acid, 320g tetraethylammonium hydroxide, 200g tetrabutylammonium hydroxide, 125g cetyltrimethylammonium bromide are added in the hydrothermal synthesis kettle, after stirring evenly, in Slowly add 20.8g tetraethyl orthosilicate dropwise under stirring state, stir evenly, then add 56g potassium hydroxide, and then seal the synthesis kettle; Aging treatment for 0.1 hour, down to room temperature, and open the lid of the kettle;

[0030] 2) After adding 0.29g of acetone, 0.3g of propanol, and 0.92g of glycerol to the synthesis solution after aging treatment, seal the synthesis kettle, and crystallize for 26 hours at a temperature of 200°C and a stirring rate of 60r / min After that, it is cooled to room temperature, discharged, washed, separated, dried and calcined to obtain a needle-shaped ZSM-11 molecular sieve with a needle-shaped cross-sectional diameter of about 3 nm.

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Abstract

The invention provides a synthesis method of a nanometer needle-like ZSM-11 and a mixed-crystal molecular sieve thereof. According to the method, the nanometer needle-like morphology of a ZSM-11 molecular sieve is realized through measures such as aging treatment of a synthetic liquid and successive addition of two synthesis assistants, and the mixed-crystal molecular sieve with the nanometer needle-like morphology containing a ZSM-11 crystal phase can be prepared by adding an induction seed crystal into the synthetic liquid. Compared with a conventional ZSM-11 molecular sieve, the ZSM-11 andthe mixed-crystal molecular sieve prepared by using the method have the advantage of obviously shorter intragranular micropore diffusion path.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves, in particular to a method for synthesizing nanoacicular ZSM-11 and mixed crystal molecular sieves. Background technique [0002] Zeolite molecular sieve is a kind of aluminosilicate crystal with regular pore (or cage) structure, which is composed of aluminum-oxygen tetrahedron and silicon-oxygen tetrahedron as basic units, which are connected to each other through bridge oxygen. Because the negative charges of the skeleton need to be balanced by cations, and there are adsorbable and desorbable water molecules in the pores (or cages), the general composition formula is generally written as [M(Ⅰ),M(II)]O·Al2O3·nSiO2·mH2O. Among them, M(I) and M(II) refer to monovalent or divalent metal cations; n is the silicon-aluminum ratio of molecular sieves, which is always greater than 1.0, that is, there is no Al-O-Al bond; m is the number of moles of adsorbed water . Because zeolite molecular sie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/36B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B39/36C01P2004/03C01P2004/62
Inventor 李军辉宋剑红龚清
Owner XIANGTAN UNIV
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