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Ultrasound-assisted superfine ERI type molecular sieve rapidly synthesizing method

An ultrasonic-assisted, molecular sieve technology, applied in separation methods, chemical instruments and methods, and dispersed particle separation, can solve the problems of shortened synthesis time, reduced synthesis cost, and long preparation time, achieving shortened synthesis time, reduced synthesis cost, and homogeneous effect

Active Publication Date: 2019-04-05
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the problems of high silicon-alumina ratio, long preparation time and expensive organic template used in existing synthetic ERI molecular sieves, the present invention combines ultrasonic treatment technology to directly water Thermally synthesized ERI type molecular sieve, which effectively avoids the use of organic templates, greatly reduces the synthesis cost, and greatly shortens the synthesis time, and at the same time can obtain low-silicon ultrafine ERI type molecular sieves with uniform shape and uniform size

Method used

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  • Ultrasound-assisted superfine ERI type molecular sieve rapidly synthesizing method
  • Ultrasound-assisted superfine ERI type molecular sieve rapidly synthesizing method
  • Ultrasound-assisted superfine ERI type molecular sieve rapidly synthesizing method

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Experimental program
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Effect test

Embodiment 1

[0039] Add TEAOH and Al[OCH(CH 3 )C 2 h 5 ] 3 , stir at room temperature until clarified, then add silicon source, then add KOH, C 12 h 3 OBr 2 N 2 , the molar ratio of each component oxide form is: n(SiO 2 ):n(Al 2 o 3 ):n(TEAOH):n(KOH):n(C 12 h 3 OBr 2 N 2 ):n(H 2 (0)=1:0.03:0.09:0.8:0.13:25 made erionite crystal seed, reaction temperature is under 150 ℃ of conditions, reacted for 5 days, the solid-liquid phase has obvious delamination after the reaction, separates the lower layer solid phase, will The solid phase was boiled, centrifuged, washed with deionized water until neutral, dried at 100°C for 12 hours, and then transferred to a muffle furnace for calcination at 550°C for 12 hours to obtain erionite seed crystals.

[0040] After dissolving aluminum hydroxide, sodium hydroxide and potassium hydroxide in sequence, after the mixed solution is clarified, add water to dilute and add silicon source. The ratio (molar ratio) of each component oxide form is: n(SiO...

Embodiment 2

[0044] Add TEAOH and Al[OCH(CH 3 )C 2 h 5 ] 3 , stir at room temperature until clarified, then add silicon source, then add KOH, C 12 h 3 OBr 2 N 2 , the molar ratio of each component oxide form is: n(SiO 2 ):n(Al 2 o 3 ):n(TEAOH):n(KOH):n(C 12 h 3 OBr 2 N 2 ):n(H 2 O)=1:0.03:0.09:0.8:0.13:25 to make erionite seed crystals, the reaction temperature is 130-180°C, react for 3-7 days, after the reaction, the solid-liquid phase has obvious stratification, and the lower layer is separated For the solid phase, boil the solid phase, centrifuge it, wash it with deionized water until neutral, dry it at 70-120°C for 5-15h, transfer it to a muffle furnace for calcination at 400-600°C for 5-15h to obtain a seed crystal.

[0045] After dissolving aluminum hydroxide, sodium hydroxide and potassium hydroxide in sequence, after the mixed solution is clarified, add water to dilute and add silicon source. The ratio (molar ratio) of each component oxide form is: n(SiO 2 ):n(Al 2 ...

Embodiment 3

[0049] Add TEAOH and Al[OCH(CH 3 )C 2 h 5 ] 3 , stir at room temperature until clarified, then add silicon source, then add KOH, C 12 h 3 OBr 2 N 2 , the molar ratio of each component oxide form is: n(SiO 2 ):n(Al 2 o 3 ):n(TEAOH):n(KOH):n(C 12 h 3 OBr 2 N 2 ):n(H 2 O)=1:0.03:0.09:0.8:0.13:25 to make erionite seed crystals.

[0050] After dissolving aluminum hydroxide, sodium hydroxide and potassium hydroxide in sequence, after the mixed solution is clarified, add water to dilute and add silicon source. The ratio (molar ratio) of each component oxide form is: n(SiO 2 ):n(Al 2 o 3 ):n(Na 2 O):n(K 2 O):n(H 2(0)=1:0.020:0.26:0.09:200, sonicated at room temperature for 60 minutes to obtain a synthetic sol. Add 0.3wt% of the prepared erionite seed crystals to the synthetic sol, the reaction temperature is 160°C, the reaction time is 24h, the solid-liquid phase of the reactant is clearly separated, the lower solid phase obtained is boiled and washed with deionize...

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Abstract

The invention provides an ultrasound-assisted superfine ERI type molecular sieve rapidly synthesizing method. The ultrasound-assisted superfine ERI type molecular sieve rapidly synthesizing method ischaracterized by comprising, in sol with no organic template, performing ultrasonic treatment for hydrothermal synthesis of pure phase low-silicon ERI type molecular sieves at 100-200 DEG C for 2-48 h, which have a grain size of 300-500 nm and a silicon-aluminum ratio of 3-4. Compared with common synthesis methods in the prior art, the ultrasound-assisted superfine ERI type molecular sieve rapidlysynthesizing method avoids application of expensive organic templates, achieves synthesis of rodlike crystals uniform in size without mechanical ageing and greatly reduces the synthesizing time. Thesynthesized ERI type molecular sieves are high in activity and thermal stability, and can serve as seed crystals for synthesizing ERI type molecular sieves or ERI type molecular sieve-enriched membranes and meanwhile as excellent catalysts for MTO (methanol to olefins) reaction. The ultrasound-assisted superfine ERI type molecular sieve rapidly synthesizing method is simple in synthetic process, low in cost, good in repeatability and easy to apply to industrial production.

Description

technical field [0001] The invention relates to a material preparation method, which belongs to the field of molecular sieve material preparation and application, in particular to a method for rapidly synthesizing ultrafine ERI molecular sieves aided by ultrasound. Background technique [0002] Erionite (ERI for short) molecular sieve structure belongs to the hexagonal crystal system, composed of cannonite cages and double six-membered rings, and has a three-dimensional eight-membered ring elliptical channel structure along the c-axis direction, with a pore size of 0.36nm×0.51nm . Due to its suitable pore size and good shape selectivity, it has been widely used in the fields of gas adsorption separation and catalysis, making the synthesis of ERI molecular sieves a research hotspot. [0003] Erionite is similar to Offretite (abbreviated as OFF) in structure and performance, and there are two positively charged cations in the 14-member super-large cage of Erionite to maintain...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/30B01D53/22
CPCB01D53/228C01B39/30C01P2002/72C01P2004/03C01P2004/62Y02C20/40Y02P20/151
Inventor 陈祥树刘义张家友胡娜刘靖张慧智桂田
Owner JIANGXI NORMAL UNIV
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