CN103073004A - Preparation method of two-dimensional layered-structure material magadiite - Google Patents
Preparation method of two-dimensional layered-structure material magadiite Download PDFInfo
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- CN103073004A CN103073004A CN2012105578682A CN201210557868A CN103073004A CN 103073004 A CN103073004 A CN 103073004A CN 2012105578682 A CN2012105578682 A CN 2012105578682A CN 201210557868 A CN201210557868 A CN 201210557868A CN 103073004 A CN103073004 A CN 103073004A
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Abstract
The invention relates to a preparation method of a two-dimensional layered-structure material magadiite. The preparation method comprises the following steps of 1, mixing a silicon source, an alkali source and water, wherein according to a mole ratio, the components of the mixture satisfy that SiO2: (NaOH+Na2CO3)=2-8; H2O: (NaOH+Na2CO3)=40-90; and NaOH: Na2CO3=1: 2, 2, putting the mixture into a closed container, and carrying out crystallization at a temperature of 130 to 190 DEG C under self-generated pressure for 6 to 72 hours, and 3, taking out crystallization products, carrying out filtration, carrying out washing until a PH value is in a range of 7-9, and drying at a temperature of 40 to 100 DEG C for 4 to 24 hours to obtain the two-dimensional layered-structure material magadiite. The preparation method has simple processes. The two-dimensional layered-structure material magadiite can be widely used as a catalyst, an adsorbent, a pillar material, an ion exchanger and a nanocomposite material filler.
Description
Technical field
The present invention relates to the preparation method of a kind of two-dimensional layered structure material magadiite.
Background technology
The laminate of two-dimensional layered structure material magadiite is by electronegative SiO
4Tetrahedron forms, preferably chemistry and thermostability are arranged, interlayer have can be exchanged the hydration sodium ion, therefore magadiite has some typical character of layered clay material, for example water and polarity organic molecule that some are little had stronger adsorptive power, has preferably swelling property between the laminate, can hold the little proton that arrives and arrive greatly high-polymer molecular or group, these character have promoted the application of magadiite as aspects such as cationite, sorbent material, pillared composite, catalyzer, nano composite material fillers.
Focus mostly on about the document of two-dimensional layered structure material magadiite at present and be compounded to form coexisting material in one or more of itself and ZSM-5, mordenite, β zeolite, ZSM-35, not yet be seen in report about the preparation of simple phase magadiite.
Summary of the invention
Technical problem to be solved by this invention is the preparation method's problem that not yet relates to two-dimensional layered structure material magadiite in the prior art, the preparation method of a kind of two-dimensional layered structure material magadiite is provided, and this two-dimensional layered structure material magadiite can be used for the aspects such as absorption, catalysis, ion-exchange.
For addressing the above problem, the technical solution used in the present invention is as follows.
The preparation method of a kind of two-dimensional layered structure material magadiite, it may further comprise the steps:
(1) silicon source, alkali source and water are mixed, satisfy with the component in the molar ratio computing mixture: SiO
2: (NaOH+Na
2CO
3)=2～8; H
2O:(NaOH+Na
2CO
3)=40～90; NaOH:Na
2CO
3=1:2; The mixture that step (1) obtains is put into encloses container under autogenous pressure, 130～190 ℃ of crystallization 6～72 hours;
(2) product that crystallization is good takes out, and after filtration, be washed to behind PH=7～9 40 ℃～100 degrees centigrade dryings 4～24 hours, makes two-dimensional layered structure material magadiite.
Further optimize, in the step (1), described silicon source is more than one in aerosil, precipitated silica, water glass, diatomite, silica gel, tetraethoxy, the methyl silicate.
Further optimize, in the step (1), described alkali source is the mixture of sodium hydroxide and yellow soda ash.
Further optimize, in the step (1), first alkali source and water are mixed into solution, and then mix with the silicon source.
Further optimize, also through grinding, make two-dimensional layered structure material magadiite after the described drying of step (3).
Compared with prior art, the present invention has following advantage and technique effect: the present invention is under the processing condition that limit, be particularly limited relative content and the crystallization process of each component in the reaction mixture, synthesized the magadiite of simple phase, preparation method's simple possible.Prepared material has two-dimensional layered structure and interlayer has tradable positively charged ion, is widely used at aspects such as ion-exchange, catalysis, absorption.
Description of drawings
Fig. 1 is the X-ray diffracting spectrum of gained two-dimensional layered structure material magadiite among the embodiment 1.
Fig. 2 is the X-ray diffracting spectrum of gained two-dimensional layered structure material magadiite among the embodiment 2.
Fig. 3 is the X-ray diffracting spectrum of gained two-dimensional layered structure material magadiite among the embodiment 3.
Fig. 4 is the X-ray diffracting spectrum of gained two-dimensional layered structure material magadiite among the embodiment 4.
Fig. 5 is the scanning electron microscope collection of illustrative plates of two-dimensional layered structure material magadiite.
Embodiment
Below by embodiment in detail the present invention is described in detail, but protection scope of the present invention is not limited to these embodiment.
Embodiment 1
Getting 0.40 gram sodium hydroxide and 2.12 gram yellow soda ash successively is dissolved in 47.52 grams and makes mixing solutions in the water, mixing solutions and 15.48 gram precipitated silicas (moisture 7wt%) are fully mixed and stirred 15 minutes, under 130 ℃, carried out hydrothermal crystallizing 72 hours in the rear adding autoclave that stirs.Product after filtration, be washed to behind PH=7～9 80 ℃ lower dry 4 hours, namely get two-dimensional layered structure material magadiite, such as Fig. 5.Carry out qualitative analysis (its X-ray diffraction spectrogram is seen accompanying drawing 1) by the X-ray diffraction method, this two-dimensional layered structure material magadiite is simple phase as can be known.
Embodiment 2
Getting 0.40 gram sodium hydroxide and 2.12 gram yellow soda ash successively is dissolved in 42.39 grams and makes mixing solutions in the water, mixing solutions and 11.61 gram precipitated silicas (moisture 7wt%) are fully mixed and stirred 15 minutes, under 150 ℃, carried out hydrothermal crystallizing 36 hours in the rear adding autoclave that stirs.Product after filtration, be washed to behind PH=7～9 80 ℃ lower dry 4 hours, namely get two-dimensional layered structure material magadiite, such as Fig. 5.Carry out qualitative analysis (its X-ray diffraction spectrogram is seen accompanying drawing 2) by the X-ray diffraction method, this two-dimensional layered structure material magadiite is simple phase as can be known.
Embodiment 3
Getting 0.40 gram sodium hydroxide and 2.12 gram yellow soda ash successively is dissolved in 37.26 grams and makes mixing solutions in the water, mixing solutions and 7.74 gram precipitated silicas (moisture 7wt%) are fully mixed and stirred 15 minutes, under 170 ℃, carried out hydrothermal crystallizing 24 hours in the rear adding autoclave that stirs.Product after filtration, be washed to behind PH=7～9 80 ℃ lower dry 4 hours, namely get two-dimensional layered structure material magadiite, such as Fig. 5.Carry out qualitative analysis (its X-ray diffraction spectrogram is seen accompanying drawing 3) by the X-ray diffraction method, this two-dimensional layered structure material magadiite is simple phase as can be known.
Getting 0.40 gram sodium hydroxide and 2.12 gram yellow soda ash successively is dissolved in 32.13 grams and makes mixing solutions in the water, mixing solutions and 3.87 gram precipitated silicas (moisture 7wt%) are fully mixed and stirred 15 minutes, under 190 ℃, carried out hydrothermal crystallizing 6 hours in the rear adding autoclave that stirs.Product after filtration, be washed to behind PH=7～9 80 ℃ lower dry 4 hours, namely get two-dimensional layered structure material magadiite, such as Fig. 5.Carry out qualitative analysis (its X-ray diffraction spectrogram is seen accompanying drawing 4) by the X-ray diffraction method, this two-dimensional layered structure material magadiite is simple phase as can be known.
Claims (5)
1. the preparation method of a two-dimensional layered structure material magadiite is characterized in that may further comprise the steps:
(1) silicon source, alkali source and water are mixed, satisfy with the component in the molar ratio computing mixture: SiO
2: (NaOH+Na
2CO
3)=2～8; H
2O:(NaOH+Na
2CO
3)=40～90; NaOH:Na
2CO
3=1:2;
(2) mixture that step (1) is obtained is put into encloses container under autogenous pressure, 130～190 ℃ of crystallization 6～72 hours;
(3) product that crystallization is good takes out, and after filtration, be washed to behind PH=7～9 40 ℃～100 degrees centigrade dryings 4～24 hours, makes two-dimensional layered structure material magadiite.
2. preparation method according to claim 1 is characterized in that in the step (1), and described silicon source is more than one in aerosil, precipitated silica, water glass, diatomite, silica gel, tetraethoxy, the methyl silicate.
3. preparation method according to claim 1 is characterized in that in the step (1), described alkali source is the mixture of sodium hydroxide and yellow soda ash.
4. preparation method according to claim 1 is characterized in that first alkali source and water being mixed into solution in the step (1), and then mixes with the silicon source.
5. preparation method according to claim 1 is characterized in that after the described drying of step (3) making two-dimensional layered structure material magadiite also through grinding.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229806A (en) * | 2014-09-10 | 2014-12-24 | 华南理工大学 | Method for synthesizing magadiite by adopting catalytic nucleation method |
| CN104445250A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | Method for synthesizing MFI type zeolite from Magadiite |
| CN109569538A (en) * | 2018-12-15 | 2019-04-05 | 华南理工大学 | A kind of environmental-protection adsorption material based on magadiite and preparation method thereof and the application in anionic dye adsorbs |
| US10781269B2 (en) | 2016-04-28 | 2020-09-22 | South China University Of Technology | Nacre-mimetic environmentally friendly composite membrane with “interpenetrating petal” structure and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101264896A (en) * | 2006-12-15 | 2008-09-17 | Ifp公司 | Method of preparing magadiite or kenyaite using an organic structuring element comprising two terminal alcohol functions |
-
2012
- 2012-12-20 CN CN2012105578682A patent/CN103073004A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101264896A (en) * | 2006-12-15 | 2008-09-17 | Ifp公司 | Method of preparing magadiite or kenyaite using an organic structuring element comprising two terminal alcohol functions |
Non-Patent Citations (1)
| Title |
|---|
| YUH-RUEY WANG ET AL.: "Hydrothermal synthesis of magadiite", 《APPLIED CLAY SCIENCE》, vol. 33, 24 March 2006 (2006-03-24), pages 73 - 77 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445250A (en) * | 2013-09-24 | 2015-03-25 | 中国石油化工股份有限公司 | Method for synthesizing MFI type zeolite from Magadiite |
| CN104445250B (en) * | 2013-09-24 | 2016-06-08 | 中国石油化工股份有限公司 | Utilize the Magadiite method synthesizing MFI type zeolite |
| CN104229806A (en) * | 2014-09-10 | 2014-12-24 | 华南理工大学 | Method for synthesizing magadiite by adopting catalytic nucleation method |
| CN104229806B (en) * | 2014-09-10 | 2018-01-16 | 华南理工大学 | A kind of method for being catalyzed nucleation process synthesis magadiite |
| US10781269B2 (en) | 2016-04-28 | 2020-09-22 | South China University Of Technology | Nacre-mimetic environmentally friendly composite membrane with “interpenetrating petal” structure and preparation method thereof |
| CN109569538A (en) * | 2018-12-15 | 2019-04-05 | 华南理工大学 | A kind of environmental-protection adsorption material based on magadiite and preparation method thereof and the application in anionic dye adsorbs |
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Application publication date: 20130501 |