Preparation method of pure nano-silicon ZSM-5 zeolite

A ZSM-5 and pure silicon technology, applied in the field of preparation of pure silicon ZSM-5 zeolite, can solve the problems of large crystal grains of pure silicon ZSM-5 zeolite, large amount of TPAOH, complicated synthesis process, etc. The effect of strong hydrophobicity and high crystallinity

Inactive Publication Date: 2013-12-11
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

[0007] The crystal grains of the pure silicon ZSM-5 zeolite synthesized in the above literature are relatively large, generally above 100nm. Although the product under some conditions is below 100nm, other auxiliary components are added during the synthesis process, which makes the synthesis process more complicated.
In addition, the above-mentioned synthetic methods all use ethyl silicate as the silicon source, and TPAOH is used as the hydrolyzing agent and the guiding agent at the same time, so that the amount of TPAOH is larger and the process is more complicated.

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  • Preparation method of pure nano-silicon ZSM-5 zeolite
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preparation example Construction

[0015] The present invention provides a kind of preparation method of nanometer pure silicon ZSM-5 zeolite, it is characterized in that, this method comprises the following steps:

[0016] 1) Organosilicate with SiO 2 According to the molar ratio of organosilicate:hydrolyzing agent:water=1:0.001-0.08:2-15, fully stir and mix with water and hydrolyzing agent, and then age for 0.3-100℃ under the condition of temperature After 48 hours, the silica gel was obtained. After drying the obtained silica gel, it was ground into silica gel particles, and the hydrolyzing agent was acid, alkali or fluorine salt;

[0017] 2) SiO 2 Meter, templating agent TPA + After mixing evenly with water according to the molar ratio of silica gel particles:template agent:water=1:0.1-1:15-40, crystallize at a temperature of 100-190°C for 1-7 days, and crystallize the resulting solid The product is calcined to obtain nano-pure silicon ZSM-5 zeolite, and the template agent is tetrapropylammonium hydroxid...

Embodiment 1

[0041] This example is used to illustrate the preparation method of nano-pure silicon ZSM-5 zeolite.

[0042] According to ethyl silicate (as SiO 2 ) : ammonium fluoride: water = 1:0.01:4 molar ratio, ammonium fluoride and ethyl silicate were successively added to water and fully stirred and mixed, the pH of the resulting mixture was 7, and then the mixture was heated at a temperature of 25 Under the condition of ℃, aging for 24 hours to obtain silica gel, the obtained silica gel was dried at 60°C and 100°C for 24 hours respectively, and then ground into 40-200 mesh silica gel particles; the obtained silica gel particles (using SiO 2 meter), template agent TPAOH and water according to SiO 2 :TPAOH:water=1:0.5:35 molar ratio after mixing evenly, dynamic crystallization at 120°C for 3 days, taking out and washing, drying at 100°C for 6 hours, and roasting at 550°C for 6 hours to obtain product Z1. Measure the relative crystallinity and average particle diameter of this product...

Embodiment 2

[0044] This example is used to illustrate the preparation method of nano-pure silicon ZSM-5 zeolite.

[0045] According to methyl silicate (as SiO 2 ) : ethylenediamine: water = 1: 0.005: 8 molar ratio, ethylenediamine and methyl silicate were successively added to water and fully stirred and mixed, the pH of the resulting mixture was 9, and then the mixture was heated at a temperature of 35 Under the condition of ℃, aging for 24 hours to obtain silica gel, the obtained silica gel was dried at 60°C and 100°C for 24 hours respectively, and then ground into 40-200 mesh silica gel particles; the obtained silica gel particles (as SiO 2 meter), templating agent (TPABr and sodium hydroxide) and water according to SiO 2 : TPABr: NaOH: water = 1: 0.2: 0.2: 20 molar ratio after mixing evenly, dynamic crystallization at 140°C for 4 days, taking out and washing, drying at 100°C for 6 hours, and roasting at 550°C for 6 hours to obtain the product Z2. Determination of the relative cryst...

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Abstract

The invention provides a preparation method of pure nano-silicon ZSM-5 zeolite, comprising the following steps: fully stirring and mixing organic silicate, water and a hydrolytic agent at the molar ratio of the organic silicate (based on SiO2) to the hydrolytic agent to water being 1:(0.001-0.08):(2-15); aging the mixture at 20-100 DEG C for 0.3-48h to obtain silicone gel; drying the silicone gel; grinding the gel into silicone gel particles; uniformly mixing the obtained silicone gel, a template and water at the molar ratio of the silicone gel particles (based on SiO2), to the template (based on TPA+) to water being 1:(0.1-1):(15-40); crystallizing at 100-190 DEG C for 1-7 days; and calcining the crystallized solid product to obtain pure nano-silicon ZSM-5 zeolite. The method is simple in step and is capable of synthesizing pure nano-silicon ZSM-5 zeolite with a crystal grain diameter less than 100nm.

Description

technical field [0001] The invention relates to a preparation method of a zeolite with an MFI structure containing only silicon element in the framework, in particular a preparation method of a nanoscale pure silicon ZSM-5 zeolite. Background technique [0002] ZSM-5 zeolite is a mesoporous zeolite with a three-dimensional intersecting pore system. Its unique pore structure provides space confinement for shape-selective catalysis on the one hand, and provides abundant access channels for reactants and products on the other hand. It provides a crystal structure basis for the preparation of industrial catalysts with high selectivity, high activity, and strong anti-coking deactivation performance, and pure silicon ZSM-5 zeolite has strong hydrophobic properties and can be used for the separation of water-insoluble organic matter It can be purified and used in the synthesis of ZSM-5 zeolites containing heteroatoms. [0003] In 1972, Mobil Corporation of the United States synthe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/38B82Y40/00
Inventor 陈亨宋家庆徐向宇
Owner BEIJING UNIV OF CHEM TECH
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