CN102225777A - Growing method of hydrotalcite with egg membrane as template - Google Patents

Growing method of hydrotalcite with egg membrane as template Download PDF

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Publication number
CN102225777A
CN102225777A CN 201110083668 CN201110083668A CN102225777A CN 102225777 A CN102225777 A CN 102225777A CN 201110083668 CN201110083668 CN 201110083668 CN 201110083668 A CN201110083668 A CN 201110083668A CN 102225777 A CN102225777 A CN 102225777A
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China
Prior art keywords
hydrotalcite
template
growth
egg
egg film
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CN 201110083668
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Chinese (zh)
Inventor
王君
李松南
景晓燕
刘琦
宋大雷
葛兰
张密林
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Harbin Engineering University
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Harbin Engineering University
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Priority to CN 201110083668 priority Critical patent/CN102225777A/en
Publication of CN102225777A publication Critical patent/CN102225777A/en
Pending legal-status Critical Current

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Abstract

The invention provides a growing method of hydrotalcite with egg membrane as a template. The method comprises the following steps of: (1) cleaning egg membrane removed from the inner surface of an egg shell; (2) preparing a mixed salt solution of divalent metal soluble salt and trivalent metal soluble salt with a divalent metal ion concentration of 0.03-3 mol/L and the molar ratio of the divalent metal ions to trivalent metal ions being 2:1-4:1, subpackaging with vials, sealing the mouth of the vial with the egg membrane and fixing to obtain a reactor; and (3) placing the reactor in an alkaline solution, nucleating and growing hydrotalcite on the surfaces of the egg membrane at the temperature of 0-60 DEG C for 0.5-100 days, filtering obtained precipitate and drying to obtain hydrotalcite. In the growing method provided by the invention, the egg membrane is used as the template to grow flower-like hydrotalcite, and other assistance conditions are not needed to be provided to help the nucleation and growth of hydrotalcite during the whole preparation process of the composite material.

Description

A kind of is the method for the growth hydrotalcite of template with the egg film
Technical field
What the present invention relates to is a kind of method of hydrotalcite.Specifically a kind of is the method for template growth hydrotalcite with the egg film.
Background technology
The special construction of hydrotalcite (LDHs) is given its diversified physicochemical property, makes it demonstrate wide application prospect in fields such as catalysis, intercalation, medicament slow release, er material, fire-retardant, sewage disposal, function luminescent material and semi-conductors.
Traditional hydrotalcite preparation method has that co-precipitation, hydro-thermal are auxiliary, roasting recovery etc.Co-precipitation generally has the following step: configuration contains the divalence and the trivalent metal salts solution of certain mol proportion; In alkaline environment, make precipitation by metallic ion ageing under 60-80 ℃ condition then, make crystal growth; At last, filter repeatedly, wash, drying promptly makes hydrotalcite.Hydro-thermal is auxiliary to be meant on the basis of co-precipitation, the precipitation that obtains is joined in the reactor, and under 120-180 ℃ condition, further ageing, crystallization.Roasting is restored and is meant " memory effect " of utilizing hydrotalcite, on the basis of co-precipitation or the auxiliary acquisition of hydro-thermal hydrotalcite, with the hydrotalcite product roasting under 400-600 ℃ condition that obtains, product of roasting is restored the process that regains hydrotalcite under certain condition.(Jun?Wang,Qi?Liu,Guangchun?Zhang,Solid?State?Sciences.1597,(11)2009;Jun?Zhu,Qiaoyun?Huang,Massimo?Pigna,Antonio?Violante,Colloids?and?SurfacesB:Biointerfaces.166,(77)2010;Yuki?Arai,Makoto?Ogawa,Applied?Clay?Science.60,(142);Fatiha?Boukraa?Djellal?Saiah,Bao-Lian?Su,Nourredine?Bettahar,Journalof?Hazardous?Materials.206,(165)2009;Yanqing?Sun,Yuming?Zhou,Zhiqiang?Wang,Xiaoyun?YeApplied?Surface?Science?6372(255)2009;A.V.Radha,P.Vishnu?Kamath,C.Shivakumara,Solid?State?Sciences.1180,7(2005))。But these traditional preparation methods are difficult to the hydrotalcite that directly acquisition has special appearance, and some special patterns can increase the specific surface area of material, and then improve the performance of material.The concentration gradient that changes reaction solution is the method that a kind of effectively direct acquisition has the material of special appearance.People such as N.Nassif utilize ammoniacal liquor or volatile salt normal temperature dispensing ammonia or ammonia and this phenomenon of carbonic acid gas, the acidic solution that will contain certain C a/P ratio is presented in the encloses container that contains ammoniacal liquor or volatile salt, make this solution under this environment, have the finite concentration gradient, thereby obtained to have the hydroxyapatite of floriform appearance.Nassif,F.Martineau,O.Syzgantseva.Chem.Mater.3653,22(2010)。
Summary of the invention
The object of the present invention is to provide a kind ofly to change the reaction solution concentration gradient, what can effectively prepare flower-shaped hydrotalcite is the method for the growth hydrotalcite of template with the egg film.
The object of the present invention is achieved like this:
(1) will clean up from the egg film that the eggshell internal surface takes off;
(2) configuration divalent-metal ion concentration is 0.03-3mol/L, divalent-metal ion and trivalent metal ion mol ratio are 2: 1-4: the mixing salt solution of the soluble salt of 1 divalent metal and the soluble salt of trivalent metal is sub-packed in the bottle, cover bottleneck, fixing with the egg film, both got reactor;
(3) described reactor is presented in the basic solution, under 0-60 ℃ condition, makes hydrotalcite, sedimentation and filtration, the drying that obtains promptly made hydrotalcite egg film surface nucleation, growth 0.5-100 days.
In order to prepare the hydrotalcite with special appearance, the invention provides a kind of is the method for the growth hydrotalcite of template with the egg film, and this method is a kind of to change the reaction solution concentration gradient, effectively prepares the method for flower-shaped hydrotalcite.
Technical characterictic of the present invention is to be the flower-shaped hydrotalcite of template growth with the egg film, need not provide other subsidiary conditions to help hydrotalcite nucleation, growth in the preparation process of whole matrix material.
Description of drawings
Fig. 1 is the XRD spectra of the hydrotalcite of being grown.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention and effect are further described.But employed concrete grammar, prescription and explanation are not limitation of the present invention.
Embodiment 1:
The egg film is taken off from the eggshell internal surface, clean up, stand-by.Configuration Mg 2+Concentration is 0.1mol/L, Mg 2+With Al 3+Mol ratio is 3: 1 Mg (NO 3) 2With Al (NO 3) 2Mixing salt solution, the solution that configures is joined in the bottle, cover bottleneck, fixing with the egg film, both reactor.This reactor is presented in the NaOH solution of 1mol/L, makes hydrotalcite nucleation, growth 7 days.The sedimentation and filtration, the drying that obtain are promptly made hydrotalcite.
Embodiment 2:
With the Mg among the embodiment 1 2+With Al 3+Mol ratio is to change into 2: 1 or 4: 1 at 3: 1, and other experiment condition can obtain the different hydrotalcites of forming of laminate with embodiment 1.
Embodiment 3:
With the Mg (NO among the embodiment 1 3) 2With Al (NO 3) 2Replace with other soluble M g and Al salt, can obtain containing the hydrotalcite of different anions intercalation.
Embodiment 4:
Can provide OH with the NaOH solution volume by volume concentration among the embodiment 1 for 30% ammoniacal liquor, 1mol/L sal volatile etc. -Solution replace and also can obtain similar product.
Used egg film can be poultry egg films such as eggshell membrane, membrane of duck egg, goose egg film in the above-mentioned fact Example.

Claims (5)

1. one kind is the method for the growth hydrotalcite of template with the egg film, it is characterized in that:
(1) will clean up from the egg film that the eggshell internal surface takes off;
(2) configuration Mg 2+Concentration is 0.03-3mol/L, Mg 2+With Al 3+Mol ratio is 2: 1-4: the mixing salt solution of the soluble salt of 1 Mg and the soluble salt of Al is sub-packed in the bottle, covers bottleneck, fixing with the egg film, has both got reactor;
(3) described reactor is presented in the basic solution, under 0-60 ℃ condition, makes hydrotalcite, sedimentation and filtration, the drying that obtains promptly made hydrotalcite egg film surface nucleation, growth 0.5-100 days.
2. according to claim 1 is the method for the growth hydrotalcite of template with the egg film, and it is characterized in that: the soluble salt of described Mg is Mg (NO 3) 2The soluble salt of described Al is Al (NO 3) 2
3. according to claim 1 and 2 is the method for the growth hydrotalcite of template with the egg film, it is characterized in that: described basic solution is the NaOH solution of 1mol/L.
4. according to claim 1 and 2 is the method for the growth hydrotalcite of template with the egg film, it is characterized in that: described basic solution is that volume by volume concentration is 30% ammoniacal liquor.
5. according to claim 1 and 2 is the method for the growth hydrotalcite of template with the egg film, and it is characterized in that: described basic solution is the 1mol/L sal volatile.
CN 201110083668 2011-04-02 2011-04-02 Growing method of hydrotalcite with egg membrane as template Pending CN102225777A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105664947A (en) * 2016-03-08 2016-06-15 济南大学 Composite NiAl-LDH/gamma-AlO(OH)/C catalyst and preparation method thereof
CN106732569A (en) * 2016-12-15 2017-05-31 哈尔滨师范大学 A kind of composite and preparation method thereof
CN108114318A (en) * 2018-01-16 2018-06-05 暨南大学 A kind of eggshell membrane/hydroxyapatite composite material and preparation method and application
CN111115667A (en) * 2020-01-02 2020-05-08 陕西科技大学 Method for growing hydrotalcite by using biomacromolecule as template

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1522794A (en) * 2003-09-05 2004-08-25 同济大学 Bionic nano superstructure material preparation method using white envelope as model
CN101766992A (en) * 2010-01-22 2010-07-07 北京化工大学 Hydrotalcite-like compound/eggshell membrane composite film and preparation method thereof
CN101979309A (en) * 2010-09-03 2011-02-23 哈尔滨工程大学 Method for preparing hydrotalcite from egg shells serving as raw material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1522794A (en) * 2003-09-05 2004-08-25 同济大学 Bionic nano superstructure material preparation method using white envelope as model
CN101766992A (en) * 2010-01-22 2010-07-07 北京化工大学 Hydrotalcite-like compound/eggshell membrane composite film and preparation method thereof
CN101979309A (en) * 2010-09-03 2011-02-23 哈尔滨工程大学 Method for preparing hydrotalcite from egg shells serving as raw material

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105664947A (en) * 2016-03-08 2016-06-15 济南大学 Composite NiAl-LDH/gamma-AlO(OH)/C catalyst and preparation method thereof
CN106732569A (en) * 2016-12-15 2017-05-31 哈尔滨师范大学 A kind of composite and preparation method thereof
CN108114318A (en) * 2018-01-16 2018-06-05 暨南大学 A kind of eggshell membrane/hydroxyapatite composite material and preparation method and application
CN108114318B (en) * 2018-01-16 2021-03-19 暨南大学 Egg membrane/hydroxyapatite composite material and preparation method and application thereof
CN111115667A (en) * 2020-01-02 2020-05-08 陕西科技大学 Method for growing hydrotalcite by using biomacromolecule as template

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Application publication date: 20111026