CN103601213A - Preparation method for low silicon-aluminum ratio nanosheet flower cluster-like mordenite molecular sieve - Google Patents
Preparation method for low silicon-aluminum ratio nanosheet flower cluster-like mordenite molecular sieve Download PDFInfo
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- CN103601213A CN103601213A CN201310650614.XA CN201310650614A CN103601213A CN 103601213 A CN103601213 A CN 103601213A CN 201310650614 A CN201310650614 A CN 201310650614A CN 103601213 A CN103601213 A CN 103601213A
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Abstract
The invention discloses a preparation method for a low silicon-aluminum ratio nanosheet flower cluster-like mordenite molecular sieve. The preparation process of the mordenite molecular sieve includes: dissolving an aluminum source and an alkali source in deionized water, adding silica sol into the obtained clarified solution to obtain a uniform white colloid, transferring the white colloid into a reaction kettle to undergo hydrothermal reaction, thus obtaining the low silicon-aluminum ratio nanosheet flower cluster-like mordenite molecular sieve. The mordenite molecular sieve prepared by the invention has the advantages of wide silicon source and aluminum source, low silicon-aluminum ratio, multiple active centers, no adding of any surfactant, low preparation cost, less environmental pollution and large specific surface area, and is conducive to spread of the reactants and product and acceleration of the reaction rate, thus being widely applicable in adsorption, separation, catalytic cracking, isomerization and other fields.
Description
Technical field
The present invention relates to a kind of low silica-alumina ratio nanometer sheet flowers shape mordenite molecular sieve preparation method, belong to mordenite molecular sieve technical field.
Background technology
Mordenite is a kind of microporous silicon aluminate of crystallization, because it has regularly arranged pore structure, and large specific surface area, the advantages such as high stability and strongly-acid, have important industrial application value in fields such as absorption, separation, catalytic cracking and isomerization.Yet due to its less aperture, when relating to macromolecular catalyzed reaction, because of the restriction of molecular diffusion rate, catalytic activity reduces greatly.For head it off, by reducing the size of particles of zeolite molecular sieve, be the zeolite molecular sieve of synthesis of nano size, improve molecule in intracrystalline rate of diffusion.
The pattern of the mordenite molecular sieve that bibliographical information is crossed at present has membranaceous, dish shape, bar-shaped, sheet etc., bibliographical information is crossed high silica alumina ratio sheet mordenite synthetic method, but also sees bibliographical information low silica-alumina ratio nanometer sheet flowers shape mordenite molecular sieve preparation method.
Summary of the invention
Order of the present invention is to provide a kind of low silica-alumina ratio nanometer sheet flowers shape mordenite molecular sieve preparation method, and it is simple that the method has process, the feature that cost is low, and prepared mordenite molecular sieve has bigger serface.
The present invention is realized by following technical proposals, and a kind of low silica-alumina ratio nanometer sheet flowers shape mordenite molecular sieve preparation method, is characterized in that comprising following process:
1) take silicon sol as silicon source, sodium metaaluminate is aluminium source, sodium hydroxide is alkali source, by silicon sol, aluminum oxide, sodium hydroxide, deionized water mol ratio, be 1.0:(0.02-0.06): (0.20-0.29): (20-70), under room temperature, first sodium metaaluminate and sodium hydroxide are joined in deionized water, stir and form homogeneous solution, in solution, slowly add silicon sol again, aging 30min under stirring at room, forms even white colloid;
2) white colloid step 1) being obtained is transferred in reactor, at temperature 160-190 ℃, carry out hydro-thermal reaction 3-7 days, the reaction product obtaining is through vacuum filtration, be less than 9 by deionized water wash to washings pH value, more than 120 ℃ of dry 12h of temperature, finally with 5 ℃/min temperature rise rate, be warming up to 550 ℃ of calcining 4-8h, obtain nanometer sheet flowers shape mordenite molecular sieve;
The invention has the advantages that prepared mordenite molecular sieve raw material adopts ,Lv source, silicon source wide material sources, silica alumina ratio is low, active centre is many, and do not add any tensio-active agent, preparation cost is cheap, and environmental pollution is low, prepared low silica-alumina ratio nanometer sheet flowers shape mordenite molecular sieve specific surface area is large, be conducive to the diffusion of reactant and resultant, accelerate speed of reaction, be widely used in the fields such as absorption, separation, catalytic cracking and isomerization.
Accompanying drawing explanation
Fig. 1 is the prepared low silica-alumina ratio nanometer sheet of embodiment 1 flowers shape mordenite molecular sieve electron-microscope scanning figure.
Fig. 2 is the prepared low silica-alumina ratio nanometer sheet of embodiment 2 flowers shape mordenite molecular sieve electron-microscope scanning figure.
Fig. 3 is the prepared low silica-alumina ratio nanometer sheet of embodiment 3 flowers shape mordenite molecular sieve electron-microscope scanning figure.
Fig. 4 is the prepared low silica-alumina ratio nanometer sheet of embodiment 4 flowers shape mordenite molecular sieve electron-microscope scanning figure.
Embodiment
Embodiment 1
1) under room temperature, first 0.8501g sodium metaaluminate and 1.6593g sodium hydroxide are joined in 46.67g deionized water, more slowly add 31.1111g silicon sol (25wt%) in solution, aging 30min under stirring at room, forms even white colloid;
2) 80.2914g white colloid step 1) being obtained is transferred in 100ml polytetrafluoro inner liner stainless steel reactor, 170 ℃ of temperature, carry out hydro-thermal reaction 4 days, the reaction product obtaining is through vacuum filtration, equal 7.5 by deionized water wash to washings pH value, more than 120 ℃ of dry 12h of temperature, finally with 5 ℃/min temperature rise rate, be warming up to 550 ℃ of calcining 6h, obtain 7.0g nanometer sheet flowers shape mordenite molecular sieve; (seeing accompanying drawing 1)
Embodiment 2
1) under room temperature, first 0.7286g sodium metaaluminate and 1.4222g sodium hydroxide are joined in 60.0g deionized water, in solution, slowly add 26.6667g silicon sol (25wt%) again, aging 30min under stirring at room, forms even 88.8175g white colloid;
2) white colloid step 1) being obtained is transferred in 100ml polytetrafluoro inner liner stainless steel reactor, 170 ℃ of temperature, carry out hydro-thermal reaction 4 days, the reaction product obtaining is through vacuum filtration, equal 7.5 by deionized water wash to washings pH value, more than 120 ℃ of dry 12h of temperature, finally with 5 ℃/min temperature rise rate, be warming up to 550 ℃ of calcining 6h, obtain 5.5g nanometer sheet flowers shape mordenite molecular sieve; (seeing accompanying drawing 2)
Embodiment 3
1) under room temperature, first 0.5829g sodium metaaluminate and 1.1378g sodium hydroxide are joined in 64.0g deionized water, in solution, slowly add 21.3333g silicon sol (25wt%) again, aging 30min under stirring at room, forms even 87.054g white colloid;
2) white colloid step 1) being obtained is transferred in 100ml polytetrafluoro inner liner stainless steel reactor, 170 ℃ of temperature, carry out hydro-thermal reaction 4 days, the reaction product obtaining is through vacuum filtration, equal 8 by deionized water wash to washings pH value, more than 120 ℃ of dry 12h of temperature, finally with 5 ℃/min temperature rise rate, be warming up to 550 ℃ of calcining 6h, obtain 4.0g nanometer sheet flowers shape mordenite molecular sieve; (seeing accompanying drawing 3)
Embodiment 4
1) under room temperature, first 0.5465g sodium metaaluminate and 1.5111g sodium hydroxide are joined in 60.0g deionized water, in solution, slowly add 26.6667g silicon sol (25wt%) again, aging 30min under stirring at room, forms even 88.7243g white colloid;
2) white colloid step 1) being obtained is transferred in 100ml polytetrafluoro inner liner stainless steel reactor, 170 ℃ of temperature, carry out hydro-thermal reaction 4 days, the reaction product obtaining is through vacuum filtration, equal 7.5 by deionized water wash to washings pH value, more than 120 ℃ of dry 12h of temperature, finally with 5 ℃/min temperature rise rate, be warming up to 550 ℃ of calcining 6h, obtain 4.5g nanometer sheet flowers shape mordenite molecular sieve; (seeing accompanying drawing 4).
Claims (1)
1. a low silica-alumina ratio nanometer sheet flowers shape mordenite molecular sieve preparation method, is characterized in that comprising following process:
1) take silicon sol as silicon source, sodium metaaluminate is aluminium source, sodium hydroxide is alkali source, by silicon sol, aluminum oxide, sodium hydroxide, deionized water mol ratio, be 1.0:(0.02-0.06): (0.20-0.29): (20-70), under room temperature, first sodium metaaluminate and sodium hydroxide are joined in deionized water, stir and form homogeneous solution, in solution, slowly add silicon sol again, aging 30min under stirring at room, forms even white colloid;
2) white colloid step 1) being obtained is transferred in reactor, at temperature 160-190 ℃, carry out hydro-thermal reaction 3-7 days, the reaction product obtaining is through vacuum filtration, be less than 9 by deionized water wash to washings pH value, more than 120 ℃ of dry 12h of temperature, finally with 5 ℃/min temperature rise rate, be warming up to 550 ℃ of calcining 4-8h, obtain nanometer sheet flowers shape mordenite molecular sieve.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229816A (en) * | 2014-09-11 | 2014-12-24 | 上海化工研究院 | Organic/inorganic complex zeolite material and preparation method thereof |
| CN106672998A (en) * | 2015-11-11 | 2017-05-17 | 中国石油化工股份有限公司 | Method for preparing small crystal lamellar mercerite |
| CN107758685A (en) * | 2016-08-23 | 2018-03-06 | 中国石油化工股份有限公司 | Nanometer aggregation piece shape modenite |
| CN112661167A (en) * | 2019-10-16 | 2021-04-16 | 中国科学院大连化学物理研究所 | Synthesis method of nano mordenite molecular sieve and molecular sieve |
| CN115536040A (en) * | 2022-09-27 | 2022-12-30 | 厦门大学 | Nano lotus leaf-shaped aluminum-rich mordenite molecular sieve, and synthesis method and application thereof |
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| JP2005112686A (en) * | 2003-10-09 | 2005-04-28 | National Institute Of Advanced Industrial & Technology | Method of manufacturing mordenite type metallosilicate |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229816A (en) * | 2014-09-11 | 2014-12-24 | 上海化工研究院 | Organic/inorganic complex zeolite material and preparation method thereof |
| CN106672998A (en) * | 2015-11-11 | 2017-05-17 | 中国石油化工股份有限公司 | Method for preparing small crystal lamellar mercerite |
| CN106672998B (en) * | 2015-11-11 | 2018-10-12 | 中国石油化工股份有限公司 | A kind of preparation method of little crystal grain sheet modenite |
| CN107758685A (en) * | 2016-08-23 | 2018-03-06 | 中国石油化工股份有限公司 | Nanometer aggregation piece shape modenite |
| CN107758685B (en) * | 2016-08-23 | 2020-09-04 | 中国石油化工股份有限公司 | Nano aggregated sheet mordenite |
| CN112661167A (en) * | 2019-10-16 | 2021-04-16 | 中国科学院大连化学物理研究所 | Synthesis method of nano mordenite molecular sieve and molecular sieve |
| CN112661167B (en) * | 2019-10-16 | 2022-11-08 | 中国科学院大连化学物理研究所 | Synthesis method of nano mordenite molecular sieve and molecular sieve |
| CN115536040A (en) * | 2022-09-27 | 2022-12-30 | 厦门大学 | Nano lotus leaf-shaped aluminum-rich mordenite molecular sieve, and synthesis method and application thereof |
| CN115536040B (en) * | 2022-09-27 | 2023-08-15 | 厦门大学 | Nano lotus leaf-shaped aluminum-rich mordenite molecular sieve, and synthetic method and application thereof |
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Application publication date: 20140226 |