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Mesoporous Zn-ZSM-5 molecular sieve and low-cost preparation method thereof

A molecular sieve and mesoporous technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, refined hydrocarbon oil, etc., can solve the problems of difficult separation, low separation efficiency, high operating cost, etc., to achieve improved dispersibility, simple synthesis method, and improved selection sexual effect

Active Publication Date: 2018-08-24
邵武绿闽环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] There is a common problem about the nanometer or small grain Zn-ZSM-5 molecular sieve above: the crystal grain of the molecular sieve is nanoscale, it is difficult to separate from the mother liquor after synthesis, and centrifugation is usually selected, which has low separation efficiency and poor operation in industrial production. high cost problem

Method used

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  • Mesoporous Zn-ZSM-5 molecular sieve and low-cost preparation method thereof
  • Mesoporous Zn-ZSM-5 molecular sieve and low-cost preparation method thereof
  • Mesoporous Zn-ZSM-5 molecular sieve and low-cost preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044] The present embodiment provides a kind of Ni-Mo / Zn-ZSM-5 catalyst, and its preparation method comprises the following steps:

[0045] 1. Preparation of mesoporous Zn-ZSM-5 molecular sieve

[0046] (1) Weigh 7.4g NaAlO 2 and 170g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 6100g of deionized water, then 200g of sulfuric acid (4mol / L) was added dropwise, 60g of TMA was added after stirring for 5min, and 1420g of water glass (containing 27.6wt% of SiO2) was added after stirring for 1h. 2 , 7.1 wt% Na 2 O and 65.3 wt% H 2 O), mixed and stirred for 4h at 30°C, the molar composition of the mixture was 0.005Al 2 o 3 :0.25Na 2 O:1SiO 2 :60H 2 O: 0.15SDA: 0.09ZnO.

[0047] (2) Heat the mixture obtained in step (1) to 70°C for aging for 4 hours, then pour the solution into a stainless steel crystallization kettle with a polytetrafluoroethylene liner, raise the temperature to 130°C for crystallization for 24 hours, and then raise the temperature to 170 ℃ static crystallizatio...

Embodiment 2

[0052] This example provides a Co-Mo / Zn-ZSM-5 catalyst, the preparation steps are the same as in Example 1, only some parameters are adjusted, as follows:

[0053] (1) Using solid silica gel as the silicon source, aluminum sulfate as the aluminum source, zinc nitrate as the zinc source, hydrochloric acid (2mol / L) as the acid source, and a mixture of pyrrole and morpholine (molar ratio 1:1) as SDA, adjust the feeding The molar ratio of its molecular sieve synthesis system is 0.02Al 2 o 3 :0.05Na 2 O:1SiO 2 :20H 2 O: 0.05SDA: 0.002ZnO.

[0054] (2) Aging conditions: 50°C, 8h; crystallization conditions: crystallization at 120°C for 12h, crystallization at 150°C for 24h, crystallization at 180°C for 24h.

[0055] (3) The solution used for the exchange is 0.5 mol / L hydrochloric acid solution, the calcination temperature is 450°C, the calcination time is 8h, and the mass fraction of impregnated zinc oxide is 12wt%.

[0056] (4) The active metal loading is 2wt% CoO and 6wt% Mo...

Embodiment 3

[0058] This example provides a Ni-Mo / Zn-ZSM-5 catalyst, the preparation steps are the same as in Example 1, only some parameters are adjusted, as follows:

[0059] (1) With solid silica gel as the silicon source, aluminum sulfate as the aluminum source, zinc chloride as the zinc source, acetic acid (6mol / L) as the acid source, and methylethylamine as SDA, the molar ratio of the molecular sieve synthesis system is adjusted to 0.03Al 2 o 3 :0.15Na 2 O:1SiO 2 :40H 2 O: 0.10SDA: 0.05ZnO.

[0060] (2) Aging conditions: 40°C, 12h; crystallization conditions: heat up in different stages, first at a heating rate of 7°C / min, 20°C is a heating section, and the processing time of the temperature section is 0.5 hours; 100 After ℃, the temperature is raised at a heating rate of 4°C / min, 10°C is a heating section, and the treatment time of the temperature section is 0.5 hours; the nucleation rate and growth rate of the crystallization process of Zn-ZSM-5 molecular sieve are treated by ...

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Abstract

The invention relates to a mesoporous Zn-ZSM-5 molecular sieve and a low-cost preparation method thereof. The diameters of mesoporouss are centralized at 5-30nm, and the specific surface area is 300-600m<2> / g; and the content of zinc oxide is 0.1-10wt% of the total weight of the molecular sieve. The mesoporous Zn-ZSM-5 molecular sieve is low in acid strength, good in dispersity of Zn and strong inanti-carbon deposition performance and can be applied to the fields of hydrocracking, catalytic cracking, hydrocarbon isomerization and the like.

Description

technical field [0001] The invention relates to the field of molecular sieve synthesis, in particular to a mesoporous Zn-ZSM-5 molecular sieve and a low-cost preparation method. Background technique [0002] Due to its special pore structure, excellent shape selectivity and hydrothermal stability, ZSM-5 molecular sieve plays an irreplaceable role in the fields of catalysis, adsorption separation, ion exchange and green chemical industry. However, due to the strong acidity of ZSM-5 molecular sieves, it is easy to produce side reactions such as cracking reactions, which limits its application in isomerization and aromatization reactions. Studies have shown that the metal modification of ZSM-5 molecular sieve can not only reduce the acidity of ZSM-5 molecular sieve, but also modify the pore structure of ZSM-5 molecular sieve. Heteroatom molecular sieves have unique catalytic properties due to the introduction of heteroatoms into the molecular sieve framework, and are widely us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40B01J29/48C10G45/12C10G45/64
CPCB01J29/405B01J29/48B01J2229/183C10G45/12C10G45/64
Inventor 岳源源杨晓亮秦鹏鲍晓军王廷海王学丽刘杰
Owner 邵武绿闽环保科技有限公司
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