Synthesis method of small-crystal-grain FER (Ferrierite) molecular sieve with laminar stacking structure

A synthesis method and molecular sieve technology, applied in the field of catalysis, can solve problems such as the agglomeration and growth of molecular sieve grains, and achieve the effects of improving surface morphology, enriching pore structure, and improving catalytic activity and stability.

Active Publication Date: 2018-11-23
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One disadvantage of this method is that, due to the higher thermal sensitivity of nano-sized molecular sieves to thermal changes, the bridging of Si-O-Si bonds will be induced under high-temperature calcination conditions, resulting in the agglomeration and growth of synthesized molecular sieve grains. effect

Method used

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  • Synthesis method of small-crystal-grain FER (Ferrierite) molecular sieve with laminar stacking structure
  • Synthesis method of small-crystal-grain FER (Ferrierite) molecular sieve with laminar stacking structure
  • Synthesis method of small-crystal-grain FER (Ferrierite) molecular sieve with laminar stacking structure

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The experimental procedure is as follows: under stirring conditions, 11.6g of alkaline silica sol, 0.175g of NaOH and 0.825g of NaAlO 2 Dissolve in 32.5mL of deionized water and mix evenly, then slowly drop into 5.10mL of ethylenediamine, stir for 1.0h and let it stand, move the obtained mixture into a polytetrafluoroethylene hydrothermal reaction kettle and seal it well, and homogeneously mix at 80°C The reactor was dynamically rotated and aged for 3 hours to form a gel; then the obtained gel was heated to 190°C for dynamic crystallization for 4 hours, and the motor rotation speed was 150rpm; after the crystallization was completed, the reactor was naturally cooled to room temperature, and the obtained solid was filtered The product was washed 3-5 times with deionized water and absolute ethanol to remove part of the Na + and template agent, and then placed in a drying oven to dry at 120°C for 6h. Move the dried molecular sieve product into a dielectric barrier dischar...

Embodiment 2

[0032] Molecular sieve preparation Referring to Example 1, 5.10 mL of ethylenediamine was replaced with 6.30 mL of pyrrolidine; the rest of the conditions were the same to prepare H-FER-Py molecular sieve. figure 1 b is the SEM image of H-FER-Py molecular sieve, the sheet thickness of the molecular sieve is 40-48nm, and the pore size distribution curve is shown in figure 2 . The evaluation conditions are the same as in Example 1, and the evaluation results are shown in Table 1.

Embodiment 3

[0034] Molecular sieve preparation Referring to Example 1, 5.10 mL of ethylenediamine was replaced with 8.75 mL of cyclohexylamine; the rest of the conditions were the same to prepare H-FER-CHA molecular sieve. figure 1 c is the SEM topography of H-FER-CHA molecular sieve, the sheet thickness of the molecular sieve is 35-65nm, and the pore size distribution curve is shown in figure 2 . The evaluation conditions are the same as in Example 1, and the evaluation results are shown in Table 1.

[0035] Table 1 Performance of FER molecular sieves synthesized by different templates to catalyze n-butene isomerization a

[0036]

[0037] a Test result of continuous reaction for 10h

[0038] Additionally, from figure 2 It can be seen from the shown pore size distribution curve that the H-FER-Py molecular sieve synthesized with Py as the template has obvious mesopore distribution in the range of 4-5nm and 20-40nm, while the H-FER-Py molecular sieve synthesized with EDA and CHA as...

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Abstract

The invention discloses a synthesis method of a small-crystal-grain FER (Ferrierite) molecular sieve with a laminar stacking structure. The synthesis method comprises the following steps: taking a silicon source, an aluminum source, alkali, an organic template agent and water as raw materials, and rotating and ageing at relatively low temperature to form initial gel; then carrying out dynamic crystallization to obtain a primary product; then removing the organic template agent under a mild condition by utilizing a lot of low-temperature plasmas generated through a dielectric barrier discharge(DBD) device, so as to obtain the small-crystal-grain FER molecular sieve with the laminar stacking structure; finally, carrying out different depths of water stream coupled low-temperature plasma treatment on the prepared molecular sieve, so as to remove framework aluminum and adjust the acidic ratio of the FER molecular sieve, and further modify the shape and structure of the molecular sieve. The molecular sieve prepared by the invention not only has good stability, but also has a very strong carbon deposition resisting capability; when the molecular sieve is used for catalyzing n-butene isomerization reaction, excellent performance is obtained, and the stability of a catalyst is effectively enhanced; the service life of the catalyst is extremely improved.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a synthesis method and application of a small-grain FER molecular sieve with a layered stacking structure. Background technique [0002] As a basic organic chemical raw material with wide application, isobutylene can be used to produce butyl rubber, polyisobutylene, tert-butanol, tert-butylamine, methyl tert-butyl ether (MTBE) and methyl methacrylate (MMA), etc. Important organic chemical products, whose demand is increasing day by day. At present, the main raw materials for the industrial production of isobutene are naphtha steam cracking to ethylene and the by-product C in the fluidized cracking unit of the refinery. 4 , and the by-product tert-butanol in the synthesis of propylene oxide by the Halcon method. [0003] At present, the industrial production methods of isobutene include isobutane dehydrogenation method, sulfuric acid extraction method, resin dehydr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04B01J29/65C07C5/27C07C11/09
CPCB01J29/65C01B39/04C01P2004/04C01P2006/17C07C5/2775C07C2529/65C07C11/09
Inventor 陈秉辉郑泓光郑进保张诺伟叶松寿
Owner XIAMEN UNIV
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