HZSM-5/SAPO-5 core-shell molecular sieve as well as preparation method and application thereof

A technology of SAPO-5 and core-shell molecular sieves, which is applied in the preparation and application of core-shell composite molecular sieve catalysts to achieve reasonable design, suppress aromatization side reactions, and solve the effect of shell phase agglomeration

Active Publication Date: 2019-01-11
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • HZSM-5/SAPO-5 core-shell molecular sieve as well as preparation method and application thereof
  • HZSM-5/SAPO-5 core-shell molecular sieve as well as preparation method and application thereof
  • HZSM-5/SAPO-5 core-shell molecular sieve as well as preparation method and application thereof

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

The invention relates to an HZSM-5 / SAPO-5 core-shell molecular sieve as well as a preparation method and an application thereof, belongs to the field of core-shell molecular sieve catalysts and provides a preparation method of the uniformly-covered HZSM-5 / SAPO-5 core-shell molecular sieve. The preparation method comprises the steps of adhering a nano-SAPO-5 molecular sieve obtained through an ionothermal method to the surface of a cation-modified HZSM-5 surface through electrostatic adsorption, roasting HZSM-5 adhered with SAPO-5 nanocrystals, feeding roasted HZSM-5 into SAPO-5 hydrothermal sol in different solid-liquid ratios, carrying out ageing, low-temperature crystallization, shock cooling and stirring, and carrying out high-temperature crystallization, so as to obtain the HZSM-5 / SAPO-5 core-shell molecular sieve. An SAPO-5 shell layer on the surface of HZSM-5 is completely covered, is uniform and compact and is provided with accumulated mesopores, and the coverage degree of the shell layer is over 95 when the core-shell solid-liquid ratio is 4 / 20-5 / 20 g / ml.

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 Applications(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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