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Hierarchical pore nano ferrierite aggregate and preparation method thereof

A ferrierite, multi-level pore technology, applied in chemical instruments and methods, molecular sieves and alkali exchange compounds, inorganic chemistry, etc., can solve the problems of low silicon and aluminum samples, large crystals, harsh crystallization conditions, etc., and achieve improved crystallization. degree, high specific surface area, and the effect of shortening the crystallization time

Active Publication Date: 2018-12-07
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Lee Y, Min B P, Kim P S, etal.Synthesis and Catalytic Behavior of Ferrierite Zeolite Nanoneedles[J].ACSCatalysis.2013,3(4):617-621 reported the use of choline as a template combined with rotational crystallization to prepare However, the crystallization conditions of this method are harsh, the silicon-aluminum ratio of the obtained sample is low, and it is easy to produce heterocrystalline phase
Kamimura Y, Kowenje C, Yamanaka K, et al.Synthesis of hydrophobic siliceousferrierite by using pyridine and sodium fluoride[J].Microporous and Mesoporous Materials.2013,181:154-159. reported a method using pyridine as template The NaF method synthesizes silicon-rich ferrierite, but the crystals obtained by this method are larger plate-like structures

Method used

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  • Hierarchical pore nano ferrierite aggregate and preparation method thereof
  • Hierarchical pore nano ferrierite aggregate and preparation method thereof
  • Hierarchical pore nano ferrierite aggregate and preparation method thereof

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preparation example Construction

[0026] The present invention also provides a method for preparing the hierarchically porous nano-ferrierite aggregate, which is characterized in that the method comprises the following steps:

[0027] (1) Fully mix the silicon source and template to obtain mixture A;

[0028] (2) Fully mix aluminum source, alkali source, water source and additives to obtain mixture B;

[0029] (3) Add the mixture B dropwise to the mixture A, and mix evenly to obtain a gel;

[0030] (4) The obtained gel is subjected to segmental dynamic crystallization, and after the crystallization is completed, the multi-level porous nano ferrierite aggregates are obtained by suction filtration, drying and roasting.

[0031] In one embodiment of the present invention, the silicon source in step (1) is water glass, silica sol (a solution with a concentration of 20-35% by weight), tetraethyl orthosilicate, white carbon black, or a mixture thereof.

[0032] In one embodiment of the present invention, the alkal...

Embodiment 1

[0058] 240g silica sol (concentration is the aqueous solution of 25% by mass) and 18g ethylenediamine are fully mixed, obtain mixture A; 6.56g sodium metaaluminate, 15.2g sodium hydroxide, 540g deionized water and 4.2g sodium fluoride are fully mixed Mix and mix for 60 minutes to obtain mixture B; add mixture B to mixture A drop by drop, and stir continuously for 3 hours until the gel is mixed evenly. The gel molar ratio is: SiO 2 : Al 2 o 3 :R:NaF:Na 2 O:H 2 O is 1:0.04:0.3:0.1:0.19:40; wherein R is ethylenediamine. Then the gel was crystallized at 70°C for 12 hours, and then crystallized at 170°C for 2 days at a rotation speed of 100 rpm. After the crystallization was completed, the hierarchical porous nano-ferrierite aggregate was obtained by suction filtration, drying, and roasting product.

[0059] figure 1 Be the XRD spectrogram of embodiment 1 gained molecular sieve, from figure 1 It can be seen that the molecular sieve obtained in this example is a pure-phase f...

Embodiment 2

[0061] 240g of silica sol (aqueous solution with a concentration of 25% by mass) and 23.7g of pyridine were fully mixed to obtain mixture A; 1.64g of sodium metaaluminate, 15.2g of sodium hydroxide, 540g of deionized water and 4.2g of sodium fluoride were fully mixed , and mixed for 50 minutes to obtain a mixture B; the mixture B was added dropwise to the mixture A, and stirred continuously for 3 hours until the gel was mixed evenly. The gel molar ratio is: SiO 2 : Al 2 o 3 :R:NaF:Na 2 O:H 2 O is 1:0.01:0.3:0.1:0.19:40; wherein R is pyridine. Then the gel was crystallized at 70°C for 12 hours, and then crystallized at 170°C for 2 days at a rotation speed of 100 rpm. After the crystallization was completed, the hierarchical porous nano-ferrierite aggregate was obtained by suction filtration, drying, and roasting product.

[0062] image 3 Be the XRD spectrogram of embodiment 2 gained molecular sieves, from image 3 It can be seen that the molecular sieve obtained in thi...

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Abstract

The invention discloses hierarchical pore nano ferrierite aggregate, characterized in that a sample of the aggregate has high degree of crystallinity; a molar ratio of SiO2 to Al2O3 is 100-1500; the particle size of particles forming the aggregate is 10-100nm; the mesoporous surface area reaches 70 square meters per gram; the mesoporous bulk volume reaches 0.12ml per gram; and the degree of crystallinity reaches 108% and is not lower than 105%. The invention further relates to a preparation method of the hierarchical pore nano ferrierite aggregate.

Description

technical field [0001] The invention relates to a multi-level porous nano ferrierite aggregate and a preparation method thereof. Background technique [0002] Ferrierite is a natural mineral with a unique two-dimensional channel structure. The ten-membered ring channel (0.42×0.54nm) and the eight-membered ring channel (0.35×0.48nm) are along the [001] and [010] directions, respectively, and The six-membered ring channels parallel to the ten-membered ring intersect with the eight-membered ring channels to form an ellipsoidal ferrierite cage. Because of its good hydrothermal stability and chemical stability, it is widely used in the petrochemical industry, especially It shows special selectivity to isobutene in n-butene skeletal isomerization, is a kind of highly shape-selective catalyst, and plays a very important role in the current industrial application of n-butene skeletal isomerization. M.S.Holm, E.Taarning, K.Egeblad et al.Catalysis with hierarchical zeolites[J].Cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/50
CPCC01B39/50C01P2006/12C01P2004/64C01P2004/03C01P2002/72
Inventor 柯明胡海强宋昭峥刘稳刘强刘洋张蕾
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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