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Method for efficiently and rapidly synthesizing H-SSZ-13 type molecular sieve

A molecular sieve, fast technology, applied in separation methods, molecular sieve catalysts, molecular sieves and base exchange compounds, etc., can solve the problem of inability to realize direct one-step synthesis of H-SSZ-13 molecular sieve, limit the industrial production of SSZ-13 molecular sieve, and complex actual process conditions And other problems, to achieve excellent catalytic activity and anti-hydrothermal aging stability, wide industrial application prospects, low price effect

Pending Publication Date: 2022-07-22
安徽纳蓝环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis process of the template is complicated, resulting in high cost of raw materials, which seriously limits the industrial production of SSZ-13 molecular sieves
In 2019, Northeastern University reported a method for rapidly synthesizing SSZ-13 zeolite molecular sieves in a patent (CN110342537A), which also uses TMAdaOH as a template to rapidly synthesize SSZ-13 molecular sieves, but the Na-SSZ-13 obtained by this method still needs H-SSZ-13 molecular sieve can only be obtained after ammonium exchange and high-temperature roasting, and it is impossible to directly synthesize H-SSZ-13 molecular sieve in one step
Patent CN108059172A discloses a preparation method of H-SSZ-13 molecular sieve, which also uses TMAdaOH as the main template agent, and simultaneously uses tetraethylammonium hydroxide, isopropylamine, etc. as auxiliary template agents, and alcohols, etc. as auxiliary solvents To achieve, the actual process conditions are complex
The above two methods all use expensive TMAdaOH as the template agent, the synthesis process is complicated, and the production cost is high, which seriously limits the practical industrial application of this type of method.

Method used

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  • Method for efficiently and rapidly synthesizing H-SSZ-13 type molecular sieve
  • Method for efficiently and rapidly synthesizing H-SSZ-13 type molecular sieve
  • Method for efficiently and rapidly synthesizing H-SSZ-13 type molecular sieve

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Effect test

Embodiment 1

[0036] A method for efficient and rapid synthesis of H-SSZ-13 type molecular sieve, comprising the following steps:

[0037] S1, the tetraethylammonium hydroxide, (NH 4 ) 2 SO 4 Add pure water in turn to mix, stir for 30 minutes to obtain a clear solution, then add aluminum sulfate, continue for 30 minutes, and stir to obtain mixed solution A;

[0038] S2. Slowly add ethyl orthosilicate to the mixed solution A obtained from S1, control the feeding time to 45min, continue stirring, age the mixed solution at 60°C for 2h, and then dry it at 100°C for 4h, and finally obtain a water-containing solution. Xerogel B with a rate of 6%;

[0039] S3. Transfer the xerogel B to a crystallization kettle with a tetrafluoroethylene lining, and use the water vapor-assisted crystallization method to raise the temperature from room temperature to 150°C at 4°C / min, and keep it for 12h;

[0040] S4. After the crystallization is completed, the crystallization kettle is cooled, the product is ta...

Embodiment 2

[0044] A method for efficient and rapid synthesis of H-SSZ-13 type molecular sieve, comprising the following steps:

[0045] S1, the benzyl trimethyl ammonium hydroxide, (NH 4 ) 2 SO 4 Add pure water in turn to mix, stir for 30 minutes to obtain a clear solution, then add aluminum sulfate, continue for 30 minutes, and stir to obtain mixed solution A;

[0046] S2. Slowly add fumed silica into the mixed solution A obtained in S1, control the feeding time to 45min, continue stirring, age the mixed solution at 60°C for 2h, and then dry it at 100°C for 4h, and finally obtain the moisture content is 6.5% xerogel B;

[0047] S3. Transfer the xerogel B to a crystallization kettle with a tetrafluoroethylene lining, and use the water vapor-assisted crystallization method to raise the temperature from room temperature to 160°C at 4°C / min, and keep it for 18h;

[0048] S4. After the crystallization is completed, the crystallization kettle is cooled, the product is taken out, the produ...

Embodiment 3

[0052] A method for efficient and rapid synthesis of H-SSZ-13 type molecular sieve, comprising the following steps:

[0053] S1, the choline chloride, NH 4 Cl was added to pure water and mixed, stirred for 30 min to obtain a clear solution, then added aluminum sulfate, continued for 30 min, and stirred to obtain mixed solution A;

[0054] S2. Slowly add the silica sol to the mixed solution A obtained in S1, control the feeding time to be 45 min, continue to stir, age the mixed solution at 60 °C for 4 hours, and then dry it at 100 °C for 4 hours, and finally obtain a water content of 6 % xerogel B;

[0055] S3. Transfer the xerogel B to a crystallization kettle with a tetrafluoroethylene lining, and use the water vapor-assisted crystallization method to raise the temperature from room temperature to 150°C at 4°C / min, and keep it for 24h;

[0056] S4. After the crystallization is completed, the crystallization kettle is cooled, the product is taken out, the product is ground a...

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Abstract

The invention discloses a method for efficiently and rapidly synthesizing an H-SSZ-13 type molecular sieve. According to the present invention, the cheap tetraethylammonium hydroxide and the like are adopted as the organic template agent to replace the expensive N, N, N,-trimethyl-1-adamantyl ammonium hydroxide, the sodium-free cation source is adopted to replace the inorganic base such as NaOH in the traditional hydrothermal crystallization method, and the solvent-free auxiliary crystallization method is adopted to efficiently and rapidly synthesize the H-SSZ-13 type molecular sieve in one step; as a solvent-free auxiliary crystallization method is adopted in the crystallization process, the crystallization process is carried out in a solution-free state, the product does not need to be filtered and washed, and no wastewater is generated in the whole process. Meanwhile, the reaction system adopts a sodium-free cation source to replace inorganic bases such as NaOH in a traditional hydrothermal crystallization method, the H-SSZ-13 molecular sieve can be obtained by roasting the product in one step, and an ion exchange step is not needed, so that the production efficiency is improved, the production cost is reduced, the generation of ammonia-nitrogen wastewater is reduced, and the method is environment-friendly.

Description

technical field [0001] The invention relates to the technical field of molecular sieve synthesis, in particular to a method for efficiently and rapidly synthesizing H-SSZ-13 type molecular sieves. Background technique [0002] Aluminosilicate zeolite SSZ-13 molecular sieve with chabazite (CHA) structure, which is composed of SiO 4 and AlO 4 The tetrahedrons are connected by oxygen bridge bonds, and are regularly arranged into eight-membered ring channels and three-dimensional intersecting channel structures. Its unique pore structure and size make it have excellent catalytic activity, high product selectivity and excellent hydrothermal stability. Therefore, it is widely used in many industrial applications such as denitration of automobile exhaust, aromatization reaction, methanol to light olefins (MTO). In recent years, in order to meet the emission reduction requirements of nitrogen oxides (NOx) in the "National VI" standard for vehicle exhaust emissions, researchers ha...

Claims

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Application Information

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IPC IPC(8): C01B39/48C01B39/02B01J29/72B01D53/94B01D53/56
CPCC01B39/48C01B39/026B01J29/723B01D53/9413C01P2002/72C01P2004/03C01P2006/37B01J2229/186B01D2258/01
Inventor 李超赵长艳查乐林田炜
Owner 安徽纳蓝环保科技有限公司