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A kind of method that utilizes fly ash to prepare multi-level porous ZSM-5 molecular sieve

A technology of ZSM-5 and fly ash, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., which can solve the problems of high impurities, low yield and crystallinity, limited diffusion speed, etc. problems, to achieve the effect of accelerating mass transfer rate, reducing economic cost and improving performance

Active Publication Date: 2022-03-08
QINGDAO UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the current problems of using fly ash to synthesize molecular sieves with many impurities, low yield and crystallinity, and limiting diffusion speed, and to provide a method for preparing multi-stage porous ZSM-5 molecular sieves using fly ash Methods

Method used

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  • A kind of method that utilizes fly ash to prepare multi-level porous ZSM-5 molecular sieve
  • A kind of method that utilizes fly ash to prepare multi-level porous ZSM-5 molecular sieve
  • A kind of method that utilizes fly ash to prepare multi-level porous ZSM-5 molecular sieve

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Embodiment 1

[0039] After calcination of 200 g of fly ash at 800 ° C, after cooling, 2000 ml of distilled water was stirred and washed 12h, filtered, dried, add 1,60 g of sodium carbonate, sufficiently ground, then put it into the muffle oven at 900 ° C Calcination 4h After cooling, calcination is calcined, and the calcined ripe as ash is laurel green, and the calcined as gray grinds the 200 mesh sieve, adding 1600 ml of 15 wt% hydrochloric acid, stirred at 80 ° C for 2 h, cooling, filtration, respectively collect the filtrate and filter residue, Filter residue was washed repeatedly to neutral, dry after drying, 650 ° C calcined 2H SiO 2 Spare, weighing 92.08g. The filtrate was added to the separatory funnel, and then the extractant was added to the separatory funnel, the volume ratio of the filtrate and the extractant was 0.8: 1, the extractant is a mixture of tributyl phosphate and benzene, and the phosphoric acid The volume ratio of butyl ester and benzene is 1: 3, and the solution in the s...

Embodiment 2

[0047] SiO 2 Al (OH) 3 Extraction method as in Example 1.

[0048] Use SiO extracted from fly ash 2 Al (OH) 3 Synthetic multi-level hole ZSM-5 molecular sieves, the use of raw material Moore ratio: SiO 2 : Al (OH) 3 : NaOH: TPABR: CTAB: H 2 O = 1: 0.017: 0.35: 0.17: 0.05: 50, according to the above-mentioned ratio, the microporous template TPABR is added to the single-mouth flask, and then the deionized water is dissolved, then sodium hydroxide provides a certain amount of alkaline environment. After dissolving, add the SIO extracted from fly ash. 2 Al (OH) 3 After stirring for 30 min, the mesh template CTAb was added, and the mixture was heated at 60 ° C, stirred 24 h to obtain gel-like substance, and the gel-like substance was shifted into the reactor with polytetrafluoroethylene liner 140. Crystallization 24 h, cooled, filtered, washed, dried, dried, and dried, dried to a muffle furnace 550 ° C.

[0049] from Figure 11 and Figure 12 As shown in the XRD and SEM map of the NA-ZSM...

Embodiment 3

[0051] SiO 2 Al (OH) 3 Extraction method as in Example 1.

[0052] Use SiO extracted from fly ash 2 Al (OH) 3 Synthetic multi-level hole ZSM-5 molecular sieves, the use of raw material Moore ratio: SiO 2 : Al (OH) 3 : NaOH: TPABR: CTAB: H 2 O = 1: 0.0125: 0.25: 0.17: 0.05: 50, according to the above-mentioned ratio, the microporous template TPABR is added to the single-mouth flask, and then the deionized water is dissolved, then sodium hydroxide is added to provide a certain basic environment. After dissolving, add the SIO extracted from fly ash. 2 Al (OH) 3 After stirring for 30 min, the mesh template CTAb was added, and the mixture was heated at 60 ° C. The gel-like substance was stirred, and the gel-like substance was moved into the reactor with the polytetrafluoroethylene liner. 180 Crystallization 48h, cooling, filtration, water washing, drying, 550 ° C for 2 h removing the template agent to obtain a Na-ZSM-5 molecular sieve.

[0053] from Figure 15 and Figure 16 As shown in ...

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Abstract

The invention discloses a method for preparing multi-level porous ZSM‑5 molecular sieves by utilizing fly ash, comprising the following steps: a. mixing fly ash and sodium carbonate for calcining to obtain calcined ash; b. adding hydrochloric acid to the calcined ash , heating and stirring, cooling and filtering, collecting the filtrate and filter residue; c, adding extractant to the filtrate to extract Al(OH) 3 ; d, the filter residue is repeatedly washed to neutrality, dried, and calcined to obtain SiO 2 E, take TPABr and dissolve it in deionized water, then add NaOH, add the above-mentioned Al(OH) prepared after dissolving 3 and SiO 2 , after stirring, add CTAB, continue stirring in a water bath to obtain a gel-like substance, cool after crystallization, filter, wash with water, dry, and calcinate to obtain Na-ZSM-5 molecular sieve. The multi-stage pore ZSM-5 molecular sieve synthesized by the present invention simultaneously introduces channels with various pore diameters inside the molecular sieve, which accelerates the mass transfer rate and improves the actual use performance.

Description

Technical field [0001] The present invention relates to the field of liquidity integrated utilization technology, and more particularly to a method of preparing a multi-stage pore ZSM-5 molecular sieve using fly ash. Background technique [0002] Fly ash is a solid residue produced by coal, and its mineral composition is very complicated, and its main mineral phases include mullish, quartz, Yili and Lingri. There are about 500 million tons of fly ash every year, and the improper treatment of fly ash will lead to serious impact, including the degradation of the soil, the harm of human health, and the environmental pollution. The fly ash particles are very suspended in the air due to its small size, and has become the main source of gas pollution. If continuous exposure to fly ash, it will cause irritation of the human organ, such as eyes, skin, nose, throat and respiratory tract, may even lead to arsenic poisoning. The dumped fly ash can reach the underground soil and ultimately r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/38
CPCC01B39/38C01P2002/72C01P2004/03C01P2002/85C01P2006/17
Inventor 钱翌张海明李龙
Owner QINGDAO UNIV OF SCI & TECH
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