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Layered nanosheet ferrierite molecular sieve as well as preparation method and application thereof

A technology of ferrierite and nano-flakes, which is applied in the direction of molecular sieves and alkali exchange compounds, molecular sieve catalysts, nanotechnology, etc., can solve the problems of high price, large sample grain size, and no record of molecular sieve application fields, etc., and achieve high selectivity, Mild crystallization conditions and long life

Pending Publication Date: 2018-11-13
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Disclosed in CN105129813A is a method for synthesizing nano-flaky ferrierite, wherein the obtained molecular sieve has a thinner flaky composition, but this method not only needs to add expensive cetyltrimethylammonium bromide and molecular sieve crystal seeds , and there is no record of the application field of the obtained molecular sieve
CN107010636A discloses a synthesis method and application of ferrierite, wherein the obtained ferrierite has good n-butene skeletal isomerization performance, but the sample crystal grains obtained by this method are relatively large, and the obtained sample needs to be acidified deal with
CN103041849B discloses a method that can increase the yield of isobutene, but the method requires the use of alkaline earth metals to modify the synthesized ferrierite

Method used

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  • Layered nanosheet ferrierite molecular sieve as well as preparation method and application thereof
  • Layered nanosheet ferrierite molecular sieve as well as preparation method and application thereof
  • Layered nanosheet ferrierite molecular sieve as well as preparation method and application thereof

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preparation example Construction

[0027] The present invention also provides a method for preparing the layered nano-sheet ferrierite molecular sieve, which is characterized in that the method comprises the following steps:

[0028] (1) Aluminum source, water source and alkali source are stirred until completely dissolved to obtain mixture A;

[0029] (2) Add the silicon source to the solution A in batches, and stir thoroughly to obtain the mixture B;

[0030] (3) adding the first template agent R1 and the second template agent R2 into the solution B, and mixing uniformly to obtain a gel;

[0031] (4) The obtained gel is subjected to segmental dynamic crystallization in a closed container, and after the crystallization is completed, the layered nano-sheet ferrierite molecular sieve is obtained through suction filtration, drying and roasting.

[0032] In one embodiment of the present invention, in step (3), the first template R1 is pyridine, pyrrole, furan, piperidine, pyrrolidine, tetrahydrofuran or cyclohexy...

Embodiment 1

[0055] Prepare layered ferrierite with the following molar composition in the gel: SiO 2 :Al 2 o 3 :R1:R2:Na 2 O:H 2 O is 30:1:9.1:0.3:6.1:1210; R1 is pyrrole, and R2 is tetraethylammonium hydroxide.

[0056] The sodium metaaluminate of 5.4g and the sodium hydroxide of 16g ​​are dissolved in the deionized water of 540g, make it dissolve completely through continuous stirring, mark as solution A; The silica sol (25% silicon dioxide) of 240g is added gradually to In solution A, stir well and mark it as solution B; add 20g of pyrrole and 5.8g of tetraethylammonium hydroxide (25% aqueous solution) into solution B, make it fully mixed, and mix for 60 minutes to obtain the desired gel. The resulting gel was aged at 70°C for 12h, and then crystallized at 170°C for 3 days. After the crystallization is completed, it is filtered by suction, dried at 120°C for 4 hours, and calcined at 550°C for 4 hours to obtain a layered nano-sheet ferrierite molecular sieve.

[0057] figure 1 B...

Embodiment 2

[0059] To prepare layered ferrierite, the molar composition of the gel is as follows: The molar composition in the gel is as follows: SiO 2 :Al 2 o 3 :R1:R2:Na 2 O:H 2 O is 33:1:13.3:0.33:8.3:1660; R1 is pyrrolidine, and R2 is tetraethylammonium hydroxide.

[0060] Dissolve 4.9g of sodium metaaluminate and 20g of sodium hydroxide in 720g of deionized water, and dissolve it completely with continuous stirring, marking it as solution A; gradually add 240g of silica sol (25% silicon dioxide) to the solution In A, stir well, marked as solution B; 28.4g of pyrrolidine and 5.8g of tetraethylammonium hydroxide (25% aqueous solution) are added in solution B, make it fully mix uniformly, mix 45 minutes, obtain the obtained Gel required. The obtained gel was aged at 70°C for 12h, and then crystallized at 170°C for 3 days. After the crystallization is completed, it is filtered by suction, dried at 120°C for 4 hours, and calcined at 550°C for 4 hours to obtain a layered nano-sheet f...

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Abstract

The invention discloses a layered nanosheet ferrierite molecular sieve. The nanosheet ferrierite molecular sieve is characterized in that the molecular sieve is a high-crystallinity pure-phase ferrierite molecular sieve; the thickness of the sheet is between 30nm to 80nm; the specific surface area is larger than or equal to 340m<2> / g; the mesoporous surface area is larger than or equal to 60 m<2> / g; the crystallinity reaches 109% or more and is larger than or equal to 106%. The invention also relates to a preparation method of the layered nanosheet ferrierite molecular sieve and application ofthe layered nanosheet ferrierite molecular sieve to alkene oligomerization, low-density polyethylene cracking and skeleton isomerization reaction in n-butene and n-pentene.

Description

technical field [0001] The invention relates to a layered nano-sheet ferrierite molecular sieve, a preparation method and application 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 channel parallel to the ten-membered ring intersects with the eight-membered ring channel to form an ellipsoidal ferrierite cage. As early as the 1970s, Plank et al. first disclosed the artificial synthesis method of ferrierite in US4016245, that is, the silicon source , aluminum source, alkali source, organic template agent and water are evenly mixed, and crystallized in an autoclave at 65°C-200°C, and then filtered, washed, dried, and roasted to obtain ferrierite. [0003] Due to its unique pore structure, good hydrothermal stability, and chemical st...

Claims

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Application Information

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IPC IPC(8): C01B39/48C01B39/04B82Y40/00B82Y30/00B01J29/65C07C5/27C07C11/09
CPCB01J29/65B82Y30/00B82Y40/00C01B39/04C01B39/48C01P2002/72C01P2004/03C01P2006/12C07C5/2737C07C11/09
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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