CN102633280A - Method for synthesising mesoporous molecular sieve by utilizing pulverized fuel ash - Google Patents

Method for synthesising mesoporous molecular sieve by utilizing pulverized fuel ash Download PDF

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Publication number
CN102633280A
CN102633280A CN2012100865426A CN201210086542A CN102633280A CN 102633280 A CN102633280 A CN 102633280A CN 2012100865426 A CN2012100865426 A CN 2012100865426A CN 201210086542 A CN201210086542 A CN 201210086542A CN 102633280 A CN102633280 A CN 102633280A
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China
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molecular sieve
hour
water
pulverized fuel
stirring
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CN2012100865426A
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Chinese (zh)
Inventor
郭红彦
何晓文
宋丽华
崔洪珊
赵星
田冬
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Huainan Normal University
Huainan Union University
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Huainan Normal University
Huainan Union University
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Priority to CN2012100865426A priority Critical patent/CN102633280A/en
Publication of CN102633280A publication Critical patent/CN102633280A/en
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Abstract

The invention provides a method for synthesising a mesoporous molecular sieve by utilizing pulverized fuel ash is disclosed and relates to a synthesis method for a molecular sieve. The synthesis method comprises the following steps of: uniformly mixing and stirring the pulverized fuel ash with a mass fraction of 36-42%, NaOH with a mass fraction of 32-36%, and NaNO3 with a mass fraction of 22-26%, milling by using a ball mill, calcining the milled materials in a muffle furnace, mixing the calcined sample with water, stirring the mixture for 24 hours at 60 DEG C, and then performing suction filtration to obtain a filtrate; weighing a small amount of CTAB (cetyltrimethyl ammonium bromide), adding deionized water, magnetically stirring until a solute is dissolved, dripping the extracted filtrate and continuing to stir, adjusting the pH value until the solution is gelatinous, transferring the gelatinous object in a high-pressure reactor containing polytetrafluoroethylene, hydrothermally crystallizing to generate a solid, then washing with distilled water, performing suction filtration, placing in a drying oven to dry, and then placing the product in a resistance furnace, heating to 550 DEG C by virtue of a program, and insulating for 30-40 minutes to obtain the product. The prices of raw materials are low, the synthesis method is simple, and the adsorption performance of the synthesised object is good.

Description

The method of the synthetic mesoporous molecular sieve of a kind of flyash
Technical field:
The present invention relates to the compound method of molecular sieve, be specifically related to the method for the synthetic mesoporous molecular sieve of a kind of flyash.
Background technology:
Mesoporous molecular sieve is a kind of novel mesopore material; It has very high absorption property, is selecting absorption, separation and catalytic field to have the potential using value, at present; Mesoporous molecular sieve adopts purifying worker raw materials such as silicon-dioxide, water glass, tetraethoxy synthetic usually; These raw materials not only cost an arm and a leg, and certain toxicity is arranged, and therefore aspect synthetic, have a very big difficult problem.
Summary of the invention:
The method that the purpose of this invention is to provide the synthetic mesoporous molecular sieve of a kind of flyash, its adopts flyash is main synthetic materials, and cost of material is cheap to be easy to get and not to have toxicity, and compound method is simple, and response procedures is easy to control, and the absorption property of synthetics is good.
In order to solve the existing problem of background technology, the present invention takes following technical scheme: its compound method is: with massfraction is flyash 36-42%, NaOH 32-36%, NaNO 3Three kinds of raw materials mix of 22-26% stir; Adopted the ball mill mill 8-12 hour; The material that mill is good is calcining 2.5-3.2 hour under 450-500 ℃ the condition in retort furnace; The sample that calcining is accomplished is that 1: 5 ratio is mixed with water by volume, and mixture is taken out rate after stirring 24 hours under 60 ℃, and it is for use to obtain filtrating;
Take by weighing a spot of CTAB, add the deionized water of certain volume, dissolved fully to solute at magnetic agitation 1-1.5 hour; The filtrating continuation that splashes into said extracted slowly stirred 1-1.5 hour, regulated pH value, until gel occurring; The immigration of blended gel object is included in the autoclave of tetrafluoroethylene, and hydrothermal crystallizing is till the solid of crystallization no longer produces at a certain temperature, and the white solid that crystallization obtains washs with zero(ppm) water; Behind B suction filtration 3 times; Place baking oven dry, place the resistance furnace program to be warming up to 550 ℃ and be incubated 30-40 minute product after dry the completion, sintering is removed template and is obtained product.
The present invention has following beneficial effect: its adopts flyash is main synthetic materials, and cost of material is cheap to be easy to get and not to have toxicity, and compound method is simple, and response procedures is easy to control, and the absorption property of synthetics is good.
Embodiment:
This embodiment is taked following technical scheme: its compound method is: with massfraction is flyash 36-42%, NaOH 32-36%, NaNO 3Three kinds of raw materials mix of 22-26% stir; Adopted the ball mill mill 8-12 hour; The material that mill is good is calcining 2.5-3.2 hour under 450-500 ℃ the condition in retort furnace; The sample that calcining is accomplished is that 1: 5 ratio is mixed with water by volume, and mixture is taken out rate after stirring 24 hours under 60 ℃, and it is for use to obtain filtrating;
Take by weighing a spot of CTAB, add the deionized water of certain volume, dissolved fully to solute at magnetic agitation 1-1.5 hour; The filtrating continuation that splashes into said extracted slowly stirred 1-1.5 hour, regulated pH value, until gel occurring; The immigration of blended gel object is included in the autoclave of tetrafluoroethylene, and hydrothermal crystallizing is till the solid of crystallization no longer produces at a certain temperature, and the white solid that crystallization obtains washs with zero(ppm) water; Behind B suction filtration 3 times; Place baking oven dry, place the resistance furnace program to be warming up to 550 ℃ and be incubated 30-40 minute product after dry the completion, sintering is removed template and is obtained product.
It is main synthetic materials that this embodiment adopts flyash, and cost of material is cheap to be easy to get and not to have toxicity, and compound method is simple, and response procedures is easy to control, and the absorption property of synthetics is good.

Claims (1)

1. the method for the synthetic mesoporous molecular sieve of a flyash, it is characterized in that its compound method is: with massfraction is flyash 36-42%, NaOH 32-36%, NaNO 3Three kinds of raw materials mix of 22-26% stir; Adopted the ball mill mill 8-12 hour; The material that mill is good is calcining 2.5-3.2 hour under 450-500 ℃ the condition in retort furnace; The sample that calcining is accomplished is that 1: 5 ratio is mixed with water by volume, and mixture is taken out rate after stirring 24 hours under 60 ℃, and it is for use to obtain filtrating;
Take by weighing a spot of CTAB, add the deionized water of certain volume, dissolved fully to solute at magnetic agitation 1-1.5 hour; The filtrating continuation that splashes into said extracted slowly stirred 1-1.5 hour, regulated pH value, until gel occurring; The immigration of blended gel object is included in the autoclave of tetrafluoroethylene, and hydrothermal crystallizing is till the solid of crystallization no longer produces at a certain temperature, and the white solid that crystallization obtains washs with zero(ppm) water; Behind B suction filtration 3 times; Place baking oven dry, place the resistance furnace program to be warming up to 550 ℃ and be incubated 30-40 minute product after dry the completion, sintering is removed template and is obtained product.
CN2012100865426A 2012-03-21 2012-03-21 Method for synthesising mesoporous molecular sieve by utilizing pulverized fuel ash Pending CN102633280A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103818920A (en) * 2013-12-24 2014-05-28 淮南师范学院 Method for preparing Si-Al ordered mesoporous molecular sieve
CN104150941A (en) * 2014-07-18 2014-11-19 西安建筑科技大学 Steel slag-based mesoporous material and preparation method thereof
CN104291349A (en) * 2014-09-26 2015-01-21 东北石油大学 Method for preparing P type molecular sieve by using coal ash as raw material
CN106492875A (en) * 2016-10-26 2017-03-15 东北农业大学 Prepare the method and the method for processing furfural waste-water of load nano-titanium dioxide/zinc oxide molecular sieves
CN112194150A (en) * 2020-11-11 2021-01-08 贵州理工学院 Preparation method of fly ash-based microporous and hierarchical porous zeolite molecular sieve

Citations (4)

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Publication number Priority date Publication date Assignee Title
CN1180044A (en) * 1996-10-15 1998-04-29 李泽民 Method for producing molecular sieve material by using flyash
CN1911800A (en) * 2006-08-31 2007-02-14 北京科技大学 Method for preparing white carbon black and pure zeolite molecular sieve using flyash
CN101100305A (en) * 2007-07-06 2008-01-09 内蒙古联合工业有限公司 Fine comprehensive utilization technique of fly ash
CN101381086A (en) * 2008-10-20 2009-03-11 西安建筑科技大学 Method for preparing Si-MCM-41 mesopore molecular sieve

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1180044A (en) * 1996-10-15 1998-04-29 李泽民 Method for producing molecular sieve material by using flyash
CN1911800A (en) * 2006-08-31 2007-02-14 北京科技大学 Method for preparing white carbon black and pure zeolite molecular sieve using flyash
CN101100305A (en) * 2007-07-06 2008-01-09 内蒙古联合工业有限公司 Fine comprehensive utilization technique of fly ash
CN101381086A (en) * 2008-10-20 2009-03-11 西安建筑科技大学 Method for preparing Si-MCM-41 mesopore molecular sieve

Non-Patent Citations (1)

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Title
吕扬等: "粉煤灰合成中孔分子筛MCM-41及其吸附性能", 《当代化工》, vol. 38, no. 5, 31 October 2009 (2009-10-31) *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103818920A (en) * 2013-12-24 2014-05-28 淮南师范学院 Method for preparing Si-Al ordered mesoporous molecular sieve
CN104150941A (en) * 2014-07-18 2014-11-19 西安建筑科技大学 Steel slag-based mesoporous material and preparation method thereof
CN104150941B (en) * 2014-07-18 2015-10-21 西安建筑科技大学 A kind of slag based mesoporous material and preparation method thereof
CN104291349A (en) * 2014-09-26 2015-01-21 东北石油大学 Method for preparing P type molecular sieve by using coal ash as raw material
CN104291349B (en) * 2014-09-26 2016-06-01 东北石油大学 A kind of take flyash as the method that P type molecular sieve prepared by raw material
CN106492875A (en) * 2016-10-26 2017-03-15 东北农业大学 Prepare the method and the method for processing furfural waste-water of load nano-titanium dioxide/zinc oxide molecular sieves
CN112194150A (en) * 2020-11-11 2021-01-08 贵州理工学院 Preparation method of fly ash-based microporous and hierarchical porous zeolite molecular sieve

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Application publication date: 20120815