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Method for preparing ZSM-5 zeolite catalyst

A zeolite catalyst, ZSM-5 technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as difficult particle size control, achieve good reproducibility, solve difficult particle size control, Easy to use effect

Inactive Publication Date: 2009-09-23
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a preparation method of ZSM-5 zeolite catalyst for the problem that the particle size is difficult to control in the preparation of ZSM-5 zeolite catalyst, and its average particle size is controlled within the range of 3-7 μm

Method used

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  • Method for preparing ZSM-5 zeolite catalyst
  • Method for preparing ZSM-5 zeolite catalyst
  • Method for preparing ZSM-5 zeolite catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Take 60ml of water glass with a modulus of 3.1 and dilute it to 200ml with deionized water to obtain solution A;

[0030] Take 11gAl 2 (SO 4 ) 3 18H 2 O, add 50ml deionized water to prepare B solution;

[0031] Under stirring, add solution B into solution A, after stirring evenly, add 1mol L dropwise -1 Sulfuric acid, adjust the pH of the system to 6±1, put the mixture in a 60°C water bath for 15 hours, then transfer it to a 500ml reaction kettle, add 0.5g tetrabutylammonium bromide, seal it, and stir at 500rpm Conditions, aging at 120°C for 4h, and then press into the mixture above the liquid surface of CO 2 gas until the system reacts to CO 2 The absorption of gas reaches saturation, and the hydrothermal crystallization is carried out at 180°C for 36h. After the crystallization is completed, it is rapidly cooled by cooling water through the cooling coil, filtered, washed, and dried to obtain the target product. The filtrate was reserved for the next repeated u...

Embodiment 2

[0034] The filtrate that obtains in embodiment 1 is through removing Na + , SO 4 2 - treatment, use it to dilute 60ml of water glass with a modulus of 3.1 to 200ml, and make A solution;

[0035] Take 11gAl 2 (SO 4 ) 3 18H 2 O, add 50ml deionized water to prepare B solution;

[0036] Under stirring, add solution B into solution A, after stirring evenly, add 1mol L dropwise-1 The pH value of the sulfuric acid adjustment system is 6±1. Under the condition of 80°C water bath, let the mixture stand for 10h, then transfer it to a 500ml reaction kettle, add 0.5g tetrabutylammonium bromide, seal it, and stir it at 700rpm aging at 140°C for 4 hours, and then inject CO over the liquid surface of the mixture 2 gas until the system reacts to CO 2 The absorption of gas reaches saturation, and the hydrothermal crystallization is carried out at 180°C for 20h. After the crystallization is completed, the catalyst is rapidly cooled by cooling water, filtered, washed and dried to obtain...

Embodiment 3

[0040] Take 70ml of water glass with a modulus of 2.8, dilute to 200ml with the filtrate after the solid-liquid separation after the previous reaction is completed, and it is A solution;

[0041] Take 3gNaAlO 2 , add 50ml of deionized water to prepare solution B; under stirring, add solution B to solution A, after stirring evenly, add 2mol·L solution dropwise -1 Nitric acid to adjust the pH value of the system to 6±1. Under the condition of 80°C water bath, let the mixture stand for 10 hours, then transfer it to a 500ml reaction kettle, add 3.0ml ethylenediamine, seal it, and under the condition of 500rpm stirring speed, in Aging at 130°C for 8h, then press into the mixture above the liquid surface of CO 2 gas until the system reacts to CO 2 The absorption of gas reaches saturation, and the hydrothermal crystallization is carried out at 180°C for 20h. After the crystallization is completed, the catalyst is rapidly cooled by cooling water, filtered, washed and dried to obtai...

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Abstract

The invention discloses a method for preparing a ZSM-5 zeolite catalyst. The method comprises the following steps: mixing mixed salt solution of a silicon source and a sodium source with aluminum salt solution according to a proportion to form silica-alumina gel, adding the silica-alumina gel and a template agent into a high-temperature high-pressure reaction kettle, and carrying out hydrothermal crystallization for the mixture under set conditions to form the ZSM-5 catalyst. The method is characterized in that during the hydrothermal crystallization, CO2 gas is introduced above the liquid level at proper time to further adjust and control the pH value of a system; during synthesis, the raw material mixing rate, crystallization temperature and crystallization time are controlled so as to effectively solve the problem of grain size control during the preparation of the ZSM-5 zeolite catalyst; and the mean grain size of the prepared zeolite catalyst is 3 to 7mu m, and the range of the grain size is 2.5 to 8mu m. The ZSM-5 zeolite catalyst prepared by the method can be used for the test of preparing cyclohexanol by cyclohexene hydration.

Description

technical field [0001] The invention relates to a ZSM-5 zeolite catalyst and a preparation method thereof. In particular, it relates to a particle size control method in the preparation process of ZSM-5 zeolite catalyst. technical background [0002] At present, the cyclohexene hydration catalyst has eliminated the early inorganic acids and ion exchange resins, and now the cyclohexene hydration production process basically uses solid molecular sieves, because they are insoluble in water, easy to separate and regenerate, and have high mechanical strength. And good heat resistance and other advantages, the most successful in industrial applications. Cyclohexene hydration reaction catalyst mostly uses ZSM-5 zeolite molecular sieve. ZSM-5 zeolite molecular sieve was first synthesized by Mobile Company in the United States in the early 1970s, and its general chemical formula is: [0003] 【M 2 (I), M(II)] O·Al 2 o 3 · nSiO2 2 mH 2 o [0004] where M 2 (I), M(II) are mono...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40B01J29/40C07C29/04C07C35/08
Inventor 金鑫张玉仙
Owner BEIJING UNIV OF CHEM TECH
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