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Method for synthesizing TS-1 zeolite through size-adjustable solvent-free method

A TS-1, solvent-free technology, applied in chemical instruments and methods, inorganic chemistry, molecular sieve compounds, etc., can solve the problems of zeolite size control difficulties, etc., and achieve the effects of reducing water pollution, complete crystal morphology, and simple operation

Pending Publication Date: 2021-06-01
QINGDAO UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because there is no addition of a large amount of solvent, it is particularly difficult to control the size of the zeolite. So far, there are few studies on the size control of the synthesized zeolite by solvent-free methods.

Method used

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  • Method for synthesizing TS-1 zeolite through size-adjustable solvent-free method
  • Method for synthesizing TS-1 zeolite through size-adjustable solvent-free method
  • Method for synthesizing TS-1 zeolite through size-adjustable solvent-free method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Put 0.60g of fumed silica and 0.81g of tetrapropylammonium hydroxide containing 0.61g of water in a mortar and grind to a particle size of 0.5 μm, then add 0.015g of pure silicalite seed crystals with an average particle size of 500nm and sulfuric acid Continue to grind 0.024g of titanium until the particle size is 0.3 μm, and then place it in a reactor for crystallization. The reaction temperature is 180°C, and the reaction time is 24h. The obtained product is suction-filtered, baked at 60°C for 24h, and calcined at 550°C for 6h to obtain TS-1 zeolite;

[0036] After XRD analysis, the TS-1 zeolite structure belongs to the MFI structure, such as figure 1 As shown, and through the SEM image, it can be seen that there are more TS-1 zeolites of about 2 μm in the crystal grains, such as image 3 As shown, the pore structure of the synthesized zeolite is microporous, such as Image 6 shown.

Embodiment 2

[0038] A method for synthesizing TS-1 zeolite by a solvent-free method of adjustable size, comprising the following steps:

[0039] Put 0.60g of fumed silica and 0.81g of tetrapropylammonium hydroxide containing 0.61g of water in a mortar and grind to a particle size of 0.6 μm, then add 0.015g of pure silicalite seed crystals with an average particle size of 200nm and sulfuric acid Continue to grind 0.024g of titanium until the particle size is 0.2μm, and then place it in a reactor for crystallization. The reaction temperature is 180°C, and the reaction time is 24h. The obtained product is subjected to suction filtration, baked at 60°C for 12h, and calcined at 550°C for 6h to obtain TS -1 zeolite;

[0040] After XRD analysis, the TS-1 zeolite structure belongs to the MFI structure, such as figure 1 As shown, the particle size distribution of the zeolite is determined to be concentrated around 850nm through the SEM image, as shown in Figure 4 shown by Image 6 The TS-1 zeol...

Embodiment 3

[0042] A method for synthesizing TS-1 zeolite by a solvent-free method of adjustable size, comprising the following steps:

[0043] 0.60g of fumed silica and 1.78g of pure silicalite seed solution (containing 0.21g of tetrapropylammonium hydroxide) and 0.024g of titanium sulfate with an average particle size of 80nm are ground to a particle size of 0.5 μm, and then loaded into the reaction In the still, after crystallization at 180°C for 24 hours, the product was suction filtered, baked at 60°C for 18 hours, and calcined at 550°C for 5 hours to obtain the product. (Because the seed crystal is too small, it is not easy to separate, so the seed crystal liquid is directly used, and the seed crystal liquid is used to adjust the size of the TS-1 zeolite by using the 80nm seed crystal in the solution.)

[0044] Its structure is consistent with the MFI structure through XRD pattern analysis, such as figure 1 shown by Figure 5 It can be seen that the particle size of the synthesize...

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Abstract

The invention discloses a method for synthesizing TS-1 zeolite through size-adjustable solvent-free method, and the method comprises the following steps of: grinding a silicon source and a water-containing organic template agent in a mortar to a particle size of 0.5-1microm, then adding a pure silica zeolite seed crystal and a titanium source, further performing grinding until the particle size is 0.1-0.5microm, then putting the mixture in a reaction kettle for crystallization reaction, and carrying out suction filtration, drying and calcining on the obtained product to obtain the TS-1 zeolite. Compared with a hydrothermal method, regulation of the particle size of the TS-1 zeolite does not need to change the proportion of the raw materials, crystallization reaction temperature and time, only the size of the pure silicon zeolite seed crystal needs to be changed, when TS-1 zeolite with different sizes is synthesized, any synthesis condition does not need to be changed, the operation is simple and safe, and the method is suitable for industrial large-scale production.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve preparation methods, and more specifically relates to a size-adjustable method for synthesizing TS-1 zeolite without a solvent. Background technique [0002] TS-1 zeolite is a microporous titanium silicalite with MFI topology with ten-membered ring straight channels and ten-membered ring zigzag channels. Since part of the silicon in the framework is replaced by titanium, it has a highly active site of four-coordinated titanium, in the presence of H 2 o 2 Or organic peroxides, which catalyze the oxidation of many hydrocarbons, including alkenes, ketones, alkanes, and organosulfur compounds, are considered to be a milestone in green catalytic oxidation. [0003] At present, TS-1 zeolite is mainly synthesized by hydrothermal method. The use of a large amount of water solvent not only reduces the space of the reactor, but also generates a large pressure, which has certain safety hazards, res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/00
CPCC01B37/005
Inventor 王磊李彬刘汉防刘艳茹肖振宇冯守华
Owner QINGDAO UNIV OF SCI & TECH
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