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Preparation method of ZSM-35 molecular sieve

A ZSM-35, molecular sieve technology, applied in the direction of iron conglomerate crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, etc., can solve the problems of increasing synthesis cost, increasing environmental treatment cost, waste of resources, etc.

Active Publication Date: 2012-08-08
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the use of organic templates not only increases the cost of synthesis, but also the traditional hydrothermal synthesis method will produce a large amount of wastewater containing high concentrations of organic templates during the washing process of molecular sieves, which not only increases the cost of environmental treatment, but also causes the cost of expensive organic templates Can not be recycled and cause a huge waste of resources

Method used

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  • Preparation method of ZSM-35 molecular sieve
  • Preparation method of ZSM-35 molecular sieve
  • Preparation method of ZSM-35 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 46.9g H in a 100ml beaker 2 O, add 7.8g sodium aluminate under stirring condition, dissolve. Add 735g of cyclohexylamine into a 2L round bottom flask, add the above-mentioned sodium aluminate solution, stir for 60 minutes, add 78.33g of fumed silica within 30 minutes, continue stirring for 120 minutes, then add 3.9g of ZSM- 35 molecular sieve seed crystals, continue to stir for 30 minutes, transfer to a 1L high-pressure reactor, and the above stirring speed is 200 rpm.

[0037] The temperature was raised to 185° C. within 6 hours, and then the reaction was stirred at a speed of 200 rpm for 12 hours. The reactor was taken out and cooled to room temperature, and the solid sample was filtered out. The solid sample was directly placed in a vacuum oven at 50°C for 24 hours to obtain the raw molecular sieve powder.

[0038] The XRD spectrum of the obtained sample is as figure 1As shown, its crystal phase is consistent with the molecular sieve obtained by the hydrotherm...

Embodiment 2

[0040] Add 46.9g H in a 100ml beaker 2 O, add 7.8g sodium aluminate under stirring condition, dissolve. Add 735g of cyclohexylamine into a 2L round bottom flask, add the sodium aluminate solution configured above, stir for 60 minutes, then add 78.33g of fumed silica within 30 minutes, continue stirring for 120 minutes and then directly transfer to 1L High-pressure reactor, the above stirring speed is 250 rpm.

[0041] The temperature was raised to 185° C. within 6 hours, and then the reaction was stirred at a speed of 250 rpm for 96 hours. The reactor was taken out and cooled to room temperature, and the solid sample was filtered out. The solid sample was directly placed in a vacuum oven at 50°C for 24 hours to obtain the original molecular sieve powder.

[0042] The XRD spectrum of the obtained sample is as image 3 As shown, its crystal phase is consistent with the molecular sieve obtained by the hydrothermal synthesis method in the prior art, showing a typical FER struct...

Embodiment 3

[0044] Add 72.4g H to a 100ml beaker 2 O, add 10.2g sodium aluminate under stirring condition, dissolve. Add 735g of cyclohexylamine into a 2L round bottom flask, add the above-mentioned aluminum sulfate solution, stir for 60 minutes, add 86.1g of 400 mesh finely ground silica gel powder within 30 minutes, and continue stirring for 120 minutes. Then 3.4g NaOH was dissolved in 7g H 2 O was added dropwise to the above reaction system, and then 15.6g of ZSM-35 molecular sieve seed crystals were added, and the stirring was continued for 30 minutes, and then transferred into a 1L high-pressure reactor, and the above stirring speeds were all 300 rpm.

[0045] The temperature was raised to 185° C. within 6 hours, and then the reaction was stirred at a speed of 300 rpm for 72 hours. The reactor was taken out and cooled to room temperature, and the solid sample was filtered out. The solid sample was directly placed in a vacuum oven at 50°C for 24 hours to obtain the original molecula...

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Abstract

The invention provides a preparation method of a ZSM-35 molecular sieve. The preparation method comprises the following steps of: firstly, with cyclohexane as a reaction medium and a template agent, adding a precursor compound of aluminum, a precursor compound of silicon, an alkali source, water and a homogeneous molecular sieve crystal seed with ZSM-35 into the cyclohexane by violent stirring to obtain a precursor mixer of the molecular sieve; crystallizing the precursor mixer prepared in the first step at the reaction temperature of 130-220DEG C for 10-240 hours; and thirdly, cooling the mixture crystallized in the second step to room temperature and filtering to obtain solid and carrying out vacuum drying on the obtained solid to obtain the ZSM-35 molecular sieve. According to the preparation method disclosed by the invention, after the synthesis is finished, the cyclohexane can be directly separated and recycled; and meanwhile, the washing of the molecular sieve is avoided and no waste water generates in the reaction. The preparation method is an environment-friendly production process for the molecular sieve.

Description

technical field [0001] The invention discloses a preparation method of ZSM-35 molecular sieve, specifically, in the presence of a small amount of water in a synthesis system of cyclohexylamine, using the template guiding effect and solvent effect of cyclohexylamine to synthesize ZSM-35 molecular sieve method. Background technique [0002] Molecular sieves are the most important family of inorganic microporous crystal materials, which have a regular pore structure (the characteristic structure can be determined by X-ray diffraction spectrum). According to the statistics of the International Zeolite Association (IZA) in 2009, the total number of molecular sieve structures has reached more than 190. [0003] Silica-alumina zeolite molecular sieve is a microporous crystal material with a strict three-dimensional lattice structure formed by connecting SiO4 tetrahedron and AlO4 tetrahedron through common oxygen atoms. Due to the peculiar pore structure characteristics of zeolite ...

Claims

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Application Information

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IPC IPC(8): C01B39/44
Inventor 李进陈季香
Owner CHINA CATALYST HLDG CO LTD
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