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ZSM-5 molecular sieve and preparation method and application thereof

A technology of ZSM-5 and molecular sieves, which is applied in chemical instruments and methods, other chemical processes, crystalline aluminosilicate zeolites, etc., can solve the difficulties in the separation of solid silicon sources, the unstable crystal form of products, and the long time required for crystallization and other problems, to achieve the effect of simple preparation process, energy utilization rate, green environmental protection, and low production cost

Pending Publication Date: 2021-12-24
INST OF PROCESS ENG CHINESE ACAD OF SCI
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Problems solved by technology

[0004] CN108862311A discloses a method for preparing a high-silicon ZSM-5 molecular sieve for VOCs degradation, which mixes silicon source, alkali source, template agent, ZSM-5 molecular sieve crystal seed with water, and then undergoes hydrothermal, sintering and ion exchange Obtain ZSM-5 molecular sieve after waiting steps, but its preparation cost is higher, preparation process is complicated
[0005] CN1057066C discloses a synthesis method of high-silicon ZSM-5 molecular sieve, which mixes raw materials such as solid silica gel, aluminum source, and organic template agent, and obtains ZSM-5 molecular sieve after hydrothermal crystallization or high-temperature aging. This preparation method Longer time required and higher production costs
[0006] CN107285339A uses tetrapropylammonium bromide or tetrapropylammonium hydroxide as a template, and adds urea as a chemical cooling agent in the synthesis system to prepare a ZSM-5 molecular sieve, which adds urea to the system to increase the synthesis cost, At the same time, the crystallinity of the product is low, and it is difficult to separate the incompletely reacted solid silicon source from the product
[0007] The above-mentioned ZSM-5 molecular sieve mostly uses chemical reagents as raw materials in the preparation process, the production cost is high, and the time required for crystallization is long, and the product has the problem of unstable crystal form

Method used

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  • ZSM-5 molecular sieve and preparation method and application thereof
  • ZSM-5 molecular sieve and preparation method and application thereof
  • ZSM-5 molecular sieve and preparation method and application thereof

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preparation example Construction

[0080] In some embodiments, after S200 and before S300, the preparation method further includes the steps of filtering, washing and drying the crystallized product in sequence.

[0081] In some embodiments, in the step of washing the crystallized product, the product is washed until the product is neutral and then dried.

[0082]In some embodiments, in the step of drying the crystallized product, the drying temperature is 80-120° C., and the drying time is 6-24 hours.

[0083] S300, sintering the crystallized product to obtain a ZSM-5 molecular sieve.

[0084] In some embodiments, the sintering temperature in step (2) is 400-600°C.

[0085] In some embodiments, the sintering time in step (2) is 4-8 hours.

[0086] In some embodiments, after S300, the preparation method further includes the following steps:

[0087] The ZSM-5 molecular sieve is pressed into tablets, ground and sieved to obtain a ZSM-5 molecular sieve of 40-60 mesh.

[0088] Yet another embodiment provides t...

Embodiment 1

[0092] This embodiment provides a kind of ZSM-5 molecular sieve and preparation method thereof, the preparation method of described ZSM-5 molecular sieve comprises the following steps:

[0093] (1) Measure 25mL of concentrated desiliconization solution, add 10.8g of silica sol to it, stir evenly, add 0.368g of sodium hydroxide and 3.5g of n-butylamine as a silicon solution, and then weigh 0.34g of Al 2 (SO 4 ) 3 18H 2 O, add water and stir to dissolve, as an aluminum solution, add the aluminum solution dropwise to the silicon solution, stir evenly, add 0.29g ZSM-5 molecular sieve seed crystals to obtain a precursor;

[0094] The molar ratio of each substance in the precursor is SiO 2 :Al 2 o 3 :Water:Na 2 O: n-butylamine=1:0.005:30:0.2:0.4, the quality of ZSM-5 molecular sieve seed crystal is 4% of the quality of ZSM-5 molecular sieve;

[0095] (2) After stirring the above precursor for 0.5h, transfer it to the reaction kettle and crystallize it in a microwave reactor a...

Embodiment 2

[0099] This embodiment provides a kind of ZSM-5 molecular sieve and preparation method thereof, the preparation method of described ZSM-5 molecular sieve comprises the following steps:

[0100] (1) Measure 25mL of concentrated desiliconization solution, add 10.8g of silica sol to it, stir evenly, add 0.368g of sodium hydroxide and 3.5g of n-butylamine as a silicon solution, and then weigh 0.20g of Al 2 (SO 4 ) 3 18H 2 O, add water and stir to dissolve, as an aluminum solution, add the aluminum solution dropwise to the silicon solution, stir evenly, add 0.29g ZSM-5 molecular sieve seed crystals to obtain a precursor;

[0101] The molar ratio of each substance in the precursor is SiO 2 :Al 2 o 3 :Water:Na 2 O: n-butylamine=1:0.003:30:0.2:0.4, the quality of ZSM-5 molecular sieve seed crystal is 4% of the quality of ZSM-5 molecular sieve;

[0102] (2) After stirring the above precursor for 0.5h, transfer it to the reaction kettle and crystallize it in a microwave reactor a...

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Abstract

The invention provides a ZSM-5 molecular sieve and a preparation method and application thereof. The preparation method comprises the steps: 1, adding desilicication liquid, an aluminum source, a template agent and ZSM-5 molecular sieve seed crystal into water and mixing to obtain a precursor, wherein the precursor comprises SiO2, Na2O, Al2O3, the template agent and water, and the molar ratio of Na2O to SiO2 is (0.05-0.4): 1; and (2) crystallizing the precursor in microwave radiation at a microwave radiation temperature greater than or equal to 140 DEG C, and sintering to obtain the ZSM-5 molecular sieve. According to the present invention, the production cost is low, the preparation process is simple, the crystallization time is short, and the prepared ZSM-5 molecular sieve has characteristics of high relative crystallinity, pure crystal phase, high specific surface area and strong adsorption.

Description

technical field [0001] The invention relates to the field of molecular sieve synthesis and solid waste recycling, in particular to a ZSM-5 molecular sieve and its preparation method and application. Background technique [0002] Molecular sieve is a crystalline silicate or aluminosilicate containing basic compounds. It has a skeleton structure formed by silicon-oxygen tetrahedrons or aluminum-oxygen tetrahedrons connected by oxygen bridges. It has good ion exchange performance and high selectivity. Adsorption performance and excellent catalytic performance. Among them, ZSM-5 molecular sieve has good thermal stability, water vapor stability and hydrophobicity, and can withstand the corrosion of other acids except HF acid, and its unique double ten-membered ring channel makes it have good shape selectivity Selectivity, and the adjustable ratio of silicon to aluminum, has a wide range of applications in the petrochemical industry, especially in the field of adsorption of volat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40B01J20/18
CPCC01B39/40B01J20/183C01P2006/16C01P2006/12C01P2002/72C01P2004/03
Inventor 孙振华李少鹏李会泉朱干宇张建波李占兵
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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