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A kind of hzsm-5/sapo-5 core-shell molecular sieve and its preparation method and application

A SAPO-5, core-shell molecular sieve technology, which is applied in the preparation and application of core-shell composite molecular sieve catalysts, achieves the effects of controlling the thickness of the shell layer, solving the agglomeration of the shell phase, and making the coating layer uniform

Active Publication Date: 2021-06-11
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Zhao Xinhong et al. (patent CN102583436A, 2016 and research paper Micropor. Mesopor. Mater., 2012, 151, 501-505) disclosed a low melting point eutectic mixture (prepared with pentaerythritol and choline chloride at a molar ratio of 1:3) In, SAPO-5 molecular sieves were prepared by microwave synthesis, and the P 2 o 5 / Al 2 o 3 , HF / Al 2 o 3 and the effects of crystallization time and crystallization temperature on the synthesis, but the prepared SAPO-5 rod-shaped crystals with an aspect ratio of 3 are 2.0×1.0μm, and there are miscellaneous peaks of AST topology and cristobalite

Method used

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  • A kind of hzsm-5/sapo-5 core-shell molecular sieve and its preparation method and application
  • A kind of hzsm-5/sapo-5 core-shell molecular sieve and its preparation method and application
  • A kind of hzsm-5/sapo-5 core-shell molecular sieve and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Synthesis of Nanometer SAPO-5 Molecular Sieves in Ion Thermal System

[0059] According to molar ratio 27 EM: 1.0 P 2 o 5 : 0.75 Al 2 o 3 : 0.25F - : 0.6 SiO 2 Preparation of nano-SAPO-5 synthetic sol, at this time the sol n (SiO 2 / P 2 o 5 ) = 0.6. Specifically: first place the low melting point eutectic mixture EM in an oil bath at 140°C until it is completely melted and appears uniform and transparent, then slowly add aluminum isopropoxide, H 3 PO 4 , acidic silica sol and hydrofluoric acid, after stirring for 0.5h, transfer it to a 100ml stainless steel crystallization kettle with a polytetrafluoroethylene liner, crystallize at 180°C for 72h under open conditions, and the product is quenched, ethanol and deionized Repeated washing with water, centrifugation, and drying at 80°C for 6 hours yielded a SAPO-5 molecular sieve, denoted as S1.

[0060] In this embodiment, the eutectic mixture with low melting point is formed by mixing and grinding pentaery...

Embodiment 2~9

[0062] Examples 2-9 According to the method and steps of Example 1, and according to the conditions in Table 1, SAPO molecular sieves were synthesized, denoted as S2-S9.

[0063] Table 1 Preparation of SAPO molecular sieves in ion thermal system

[0064]

Embodiment 10

[0066] (1) Surface pretreatment of nuclear phase molecular sieve HZSM-5

[0067] Put HZSM-5 molecular sieve in 1 wt.%~30 wt.% cationic reagent aqueous solution according to the solid-liquid ratio of 1:100 (g / ml), stir in a water bath at 40~60°C for 40 min, quench with ice water, and filter with suction , and dried at 80°C for 8 h to obtain HZSM-5(PDDA) with a positive surface charge, which was designated as HZSM-5-Ι.

[0068] (2) HZSM-5-Ι adheres to SAPO-5 crystallites

[0069] Under the condition of 30°C water bath, put the nano-SAPO-5 molecular sieve prepared in Example 1 into the deionized water according to the mass ratio of 1:200 to the deionized water, and ultrasonically disperse for 30min to obtain a mixed solution, and then HZSM-5 -I molecular sieves are put into the mixed solution according to the mass ratio of HZSM-5 and nano-SAPO-5 as 1:3, continue to ultrasonic for 5~10min, let stand, adhere to microcrystals for 3h, wash, suction filter, dry at 100°C for 6h, and ...

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Abstract

HZSM-5 / SAPO-5 core-shell molecular sieve and its preparation method and application belong to the field of core-shell type composite molecular sieve catalysts, and provide a preparation method for uniformly coated HZSM-5 / SAPO core-shell molecular sieve, which is obtained by ionothermal method SAPO-5 molecular sieves are adhered to the surface of cation-modified HZSM-5 through electrostatic adsorption, and then the HZSM-5 adhered to SAPO-5 nanocrystals is fired and put into the hydrothermal sol of SAPO-5 according to different solid-to-liquid ratios , through aging, low-temperature crystallization, quenching, stirring, and then crystallization at high temperature to obtain HZSM-5 / SAPO-5 core-shell molecular sieve. The SAPO-5 shell on the HZSM-5 surface of the present invention is completely covered, uniform and dense, and contains stacked mesopores. When the core-shell solid-liquid ratio is 4 / 20~5 / 20 g / ml, the shell coverage is greater than 95 %.

Description

technical field [0001] The invention belongs to the technical field of preparation and application of core-shell type composite molecular sieve catalysts, and specifically relates to a method for preparing HZSM-5 / SAPO-5 core-shell molecular sieves by adhering microcrystal two-stage method, and the invention also relates to the prepared core Application of shell molecular sieves in the aromatization of isobutane. Background technique [0002] With the increasing scarcity of petroleum resources, the efficient use of low-carbon hydrocarbon resources has become a research hotspot, among which low-carbon hydrocarbon aromatization technology can use low-carbon hydrocarbons from a wide range of sources and relatively low prices to prepare benzene, toluene, ethylbenzene and xylene ( BTEX) and other important chemical raw materials have broad development prospects. [0003] The aromatization reaction of low-carbon hydrocarbons on solid acid catalysts is a catalytic reaction under th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/85B01J37/10B01J37/08B01J37/34C01B39/54C01B39/04C07C2/84C07C15/04C07C15/06C07C15/073C07C15/08
CPCB01J29/85B01J35/0073B01J37/0018B01J37/10B01J37/343C01B39/04C01B39/54C07C2/84C07C15/04C07C15/06C07C15/073C07C15/08Y02P20/52
Inventor 张瑞珍王志翔
Owner TAIYUAN UNIV OF TECH
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