Preparation method for nanometer flaky ferrierite molecular sieve

A ferrierite and nano-sheet technology, which is applied in the field of zeolite molecular sieve synthesis, can solve the problems of large amount of template agent, narrow silicon-aluminum ratio range, limited reduction of molecular sieve particle size, etc., and achieves wide synthesis phase area and simple synthesis method. , the prospect of industrial application has a significant effect

Active Publication Date: 2015-12-09
EAST CHINA NORMAL UNIV
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  • Abstract
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Problems solved by technology

The disadvantage of this method is that the applicable silicon-aluminum ratio is narrower (SiO 2 / Al 2 o 3 =18.5-28.6), the amount of template agent is larger (template agent / SiO 2 =0.81-1.25), and the particle size reduction of the resulting molecular sieve is limited (greater than 0.5 microns)

Method used

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  • Preparation method for nanometer flaky ferrierite molecular sieve
  • Preparation method for nanometer flaky ferrierite molecular sieve
  • Preparation method for nanometer flaky ferrierite molecular sieve

Examples

Experimental program
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Embodiment 1

[0019] Dissolve 4.45 grams of aluminum sulfate octadecahydrate and 1.18 grams of concentrated sulfuric acid in 70 grams of water, slowly add the obtained solution dropwise to 53.4 grams of water glass (silica content 22.5wt%; sodium oxide content 6.7wt%), and then add 5.96 grams of piperidine are structure-directing agents and 3.644 grams of cetyltrimethylammonium bromide (CTABr), SiO in the synthesis system 2 / Al 2 o 3 The molar ratio is 30; Na 2 O / SiO 2 The molar ratio is 0.13; H 2 O / SiO 2 The molar ratio is 30; piperidine / SiO 2 The molar ratio is 0.35; CTABr / SiO 2 The molar ratio was 0.05, and the synthetic system was stirred at room temperature for 2 hours, then at 150 o The crystallization reaction was carried out at a temperature of C for 5 days, and after the reaction was completed, the product was filtered and dried to obtain a nano-flaky ferrierite molecular sieve.

[0020] See attached figure 1 , The product obtained in Example 1 is measured by XRD and its c...

Embodiment 2

[0024] 0.53 gram of sodium hydroxide and 1.90 gram of sodium metaaluminate (aluminum oxide mass content 53.6%, sodium oxide mass content 43.8%) were dissolved in 36 grams of water, then 4.65 gram of hexamethylenediamine was added as structure directing agent, 12.72 gram of Qingdao silica gel ( Solid content 94.6%) and 7.29 grams of cetyltrimethylammonium bromide (CTABr), SiO in the synthesis system 2 / Al 2 o 3 The molar ratio is 20; Na 2 O / SiO 2 The molar ratio is 0.10; H 2 O / SiO 2 The molar ratio is 10; Hexamethylenediamine / SiO 2 The molar ratio is 0.2; CTABr / SiO 2 The molar ratio was 0.1, and the synthesis system was stirred at room temperature for 3 hours, then at 150 o The crystallization reaction was carried out at a temperature of C for 5 days, and after the reaction was completed, the product was filtered and dried to obtain a nano-flaky ferrierite molecular sieve.

[0025]The crystal phase of the obtained product was measured by XRD as FER topological structure...

Embodiment 3

[0026] 1.06 grams of sodium hydroxide and 0.95 grams of sodium metaaluminate (alumina mass content 53.6%, sodium oxide mass content 43.8%) were dissolved in 12 grams of water, and the solution obtained was slowly added dropwise to 53.4 grams of water glass (silicon oxide content 22.5wt%; sodium oxide content 6.7wt%), then add 0.032 grams of pyridine as a structure-directing agent, 20 grams of silica sol (silicon oxide 30%) as a silicon source and 0.073 grams of cetyltrimethylammonium bromide ( CTABr); SiO in the synthesis system 2 / Al 2 o 3 The molar ratio is 40; Na 2 O / SiO 2 The molar ratio is 0.10; H 2 O / SiO 2 The molar ratio is 15; pyridine / SiO 2 The molar ratio is 0.02; CTABr / SiO 2 The molar ratio was 0.01, and the synthesis system was stirred at room temperature for 3 hours, then at 160 o The crystallization reaction was carried out at a temperature of C for 2 days, and after the reaction was completed, the product was filtered and dried to obtain a nano-flaky fer...

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Abstract

The invention discloses a preparation method for a nanometer flaky ferrierite molecular sieve. The preparation method is characterized by comprising the following steps: mixing an inorganic silicon source, an aluminum source and an alkali source with pyridine, piperidine, piperazine, tetrahydrofuran or hexylenediamine; then introducing cetyl trimethyl ammonium bromide (CTABr) and carrying out stirring at room temperature for 1 to 3 h; then carrying out a crystallization reaction at 120 to 180 DEG C for 2 and 10 d; and after completion of the reaction, carrying out filtering and drying so as to obtain the nanometer flaky ferrierite molecular sieve. Compared with the prior art, the nanometer flaky ferrierite molecular sieve prepared in the invention has a great outer specific surface area, a high accumulation mesopore volume as high as 0.88 ml / g and a flake thickness of less than 10 nanometers; and the preparation method has the advantages of easiness, mild reaction conditions, a wide synthesis phase, capacity of preparing pure-phase ferrierite in a wide range of a silica-alumina ratio, high yield of ferrierite, certain industrialization prospects and substantial economic values.

Description

technical field [0001] The invention relates to the technical field of zeolite molecular sieve synthesis, in particular to a method for preparing nano-flaky ferrierite molecular sieves. Background technique [0002] Ferrierite has a FER topology and was first developed by the Mobil Petroleum Company of the United States in the 1970s (US4016245). Ferrierite has a two-dimensional channel structure of ten-membered ring channels (0.42×0.54nm) along the [001] direction and eight-membered rings (0.35×0.48nm) along the [010] direction. There is a small ellipsoidal cage at the intersection of the six-membered ring channel and the eight-membered ring channel, that is, the FER cage. Ferrierite has good catalytic activity in many hydrocarbon conversion processes such as isomerization, cracking, polymerization aromatization and other olefin skeletal isomerization, and has a wide range of industrial application prospects. Ferrierite can be synthesized by using pyridine, piperidine, eth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 薛腾吴海虹吴鹏何鸣元
Owner EAST CHINA NORMAL UNIV
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