Preparation method of SSZ-13 molecular sieve composite material

A 1. SSZ-13, composite material technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problems of no mass production, high price, limited prospects, etc., and achieve an improved ratio. Effects of surface area and pore volume, lower production costs, and improved solubility

Active Publication Date: 2022-06-24
山东泓泰恒瑞新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the templates used in the synthesis of SSZ-13 molecular sieves are N,N,N,-trimethyl-1-adamantyl ammonium hydroxide cation, benzyltri Methylammonium cation or hydroxide-N,N-dimethyl-3,5-dimethylpiperidine are used as templates, but these three templates are expensive, and about 1.2 tons are needed to produce one ton of SSZ-13 molecular sieve - 2.4 tons of the above-mentioned template agent, but there are very few domestic manufacturers capable of industrial production, resulting in the high cost of synthesizing SSZ-13 molecular sieve, which seriously limits its industrial production
[0004] The prior art discloses the use of choline chloride or other templates to synthesize SSZ-13 molecular sieves, but choline chloride is unstable under alkaline conditions It is easy to decompose into trimethylamine, ethylene glycol, etc. at high temperature, resulting in the defect of the final SSZ-13 molecular sieve, resulting in a large consumption of template agent and extremely low yield, and the product failure rate is extremely high, so the prospect is limited
[0005]Therefore, the SSZ-13 molecular sieve has a long reaction cycle and a relatively low yield, and the key raw material template agent is used in a large amount and is expensive. There is no mass production in China, so the production The production cost of SSZ-13 molecular sieve remains high

Method used

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  • Preparation method of SSZ-13 molecular sieve composite material
  • Preparation method of SSZ-13 molecular sieve composite material
  • Preparation method of SSZ-13 molecular sieve composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Synthesis of SSZ-13 molecular sieve seeds:

[0049] (1-1) Weigh the material according to the aluminum source, silicon source, sodium hydroxide, organic amine template agent (R) and water according to the molar ratio of 0.025:1:0.15:0.35:30, and first mix the aluminum source and hydrogen peroxide with water. Sodium was dissolved, stirred for 10 minutes, then added organic amine template (R) and stirred for 1 hour, finally added silicon source and stirred for 6 hours, put it into a reactor with a filling degree of 60%, and crystallized at 150 ° C for 72 hours.

[0050] (1-2) After the reaction, the product is separated by centrifugation or suction filtration, the supernatant liquid is poured off, the remaining solids are continuously added with deionized water, centrifuged after ultrasonication for 10 minutes, and the supernatant liquid is poured out.

[0051] (1-3) Repeat step (2) 3 times until the pH of the supernatant is between 7-8, to obtain solid SSZ-13 molecul...

Embodiment 2

[0062] (1) Synthesis of SSZ-13 molecular sieve seeds:

[0063] (1-1) Weigh the material according to the aluminum source, silicon source, sodium hydroxide, organic amine template agent (R) and water according to the molar ratio of 0.025:1:0.15:0.35:30, and first mix the aluminum source and hydrogen peroxide with water. Sodium was dissolved, stirred for 10 minutes, then added organic amine template (R) and stirred for 1 hour, finally added silicon source and stirred for 6 hours, put it into a reactor with a filling degree of 60%, and crystallized at 170 ° C for 120 hours.

[0064] (1-2) After the reaction, the product was separated by suction filtration, the supernatant liquid was poured off, the remaining solids were continuously added with deionized water, centrifuged after ultrasonication for 10 min, and the supernatant liquid was poured out.

[0065] (1-3) Repeat step (2) 4 times until the pH of the supernatant is between 8, to obtain solid SSZ-13 molecular sieve, dry at 90...

Embodiment 3

[0076] (1) Synthesis of SSZ-13 molecular sieve seeds:

[0077] (1-1) Weigh the materials according to the aluminum source, silicon source, sodium hydroxide, organic amine template agent (R) and water according to the molar ratio of 0.033:1:0.2:0.3:30. Sodium was dissolved, stirred for 10 minutes, then added organic amine template (R) and stirred for 1 hour, finally added silicon source and stirred for 6 hours, put it into a reactor with a filling degree of 60%, and crystallized at 150 ° C for 72 hours.

[0078] (1-2) After the reaction, the product is separated by centrifugation or suction filtration, the supernatant liquid is poured off, the remaining solids are continuously added with deionized water, centrifuged after ultrasonication for 10 minutes, and the supernatant liquid is poured out.

[0079] (1-3) Step (2) was repeated 4 times until the pH of the supernatant liquid was between 8 to obtain solid SSZ-13 molecular sieve, which was dried at 100° C. and ground to obtain ...

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Abstract

The invention belongs to the field of molecular sieve synthesis, and particularly relates to a preparation method of an SSZ-13 molecular sieve composite material. The preparation method of the SSZ-13 molecular sieve composite material comprises the following steps: synthesizing an SSZ-13 molecular sieve seed crystal; pretreating halloysite; and synthesizing the SSZ-13 molecular sieve composite material. According to the method, the pretreated halloysite is added into the SSZ-13 growth solution for crystallization reaction, so that the yield is increased, and the production cost is greatly reduced; the SSZ-13 molecular sieve composite material obtained by the invention has the property of a hierarchical porous structure, the porosity of a molecular sieve and a catalyst can be improved, and the yield and the catalytic performance are improved.

Description

technical field [0001] The invention belongs to the field of molecular sieve synthesis, in particular to a preparation method of SSZ-13 molecular sieve composite material. Background technique [0002] SSZ-13 molecular sieve is a molecular sieve with CHA topology, which is composed of AlO 4 and SiO 4 Tetrahedrons are connected end-to-end by oxygen atoms to form an ellipsoid cage with an eight-membered ring structure and a three-dimensional crossed channel structure. The channel size is 0.38nm×0.38nm. SSZ-13 molecular sieve is mainly used in the removal of NOx from automobile exhaust, methanol to light olefins (MTO) and gas separation and adsorption, and it shows good performance. [0003] At present, the template agents used in the synthesis of SSZ-13 molecular sieves are N,N,N,-trimethyl-1-adamantylammonium hydroxide cation, benzyltrimethylammonium cation or hydroxide-N,N-dimethylammonium hydroxide -3,5-Dimethylpiperidine is the template agent, but these three template a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04B01J29/76B01J29/70
CPCC01B39/04B01J29/7015B01J29/763C01P2002/72C01P2004/03C01P2006/12B01J2229/18
Inventor 张冬冬田涛马殿民孙建刚王磊张纪涛王忠邱勇马冉
Owner 山东泓泰恒瑞新材料有限公司
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