CN104944431B - A kind of inorganic supermolecule electric double layer two-dimensional nano piece and preparation method thereof - Google Patents
A kind of inorganic supermolecule electric double layer two-dimensional nano piece and preparation method thereof Download PDFInfo
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- CN104944431B CN104944431B CN201510313327.9A CN201510313327A CN104944431B CN 104944431 B CN104944431 B CN 104944431B CN 201510313327 A CN201510313327 A CN 201510313327A CN 104944431 B CN104944431 B CN 104944431B
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Abstract
The present invention relates to a kind of inorganic supermolecule electric double layer two-dimensional nano piece and preparation method thereof, the raw material based on montmorillonite or class montmorillonite, inorganic supermolecule electric double layer two-dimensional nano piece has been obtained by steps such as Delamination colloidization, colloidal coagulations, the nanometer sheet can be widely applied to the fields such as catalysis, sewage disposal, anticorrosive paint, with good application prospect.
Description
Technical field
The present invention relates to a kind of inorganic supermolecule electric double layer two-dimensional nano piece and preparation method thereof, belong to inorganic nano material
Preparing technical field.
Background technology
The montmorillonite or class montmorillonite of cationic layer structure, are 2:The lamellar aluminosilicate of 1 type, its structure composition can
It is written as：Na0.66(OH)4Si8(Al3.34Mg0.66)O20, its feature structure is the 2 of XRD spectraθPeak includes 6.0 °+1.0°、
20.0°+1.0°、35.0°+1.0°、60.0°+1.0°.The unit cell of montmorillonite is by two panels drift angle Si-O tetrahedrons inwardly
Press from both sides the octahedra layer structures for being formed of a piece of Al-O or Mg-O.Montmorillonite or class montmorillonite by electronegative laminate and interlayer sun from
Son composition, the laminate of the negatively charged has good stability and certain rigidity, is the chip for being capable of stable existence.
Class montmorillonite can be prepared using hydro-thermal method, and its raw material is waterglass, Al (NO3)3 .9H2O、Mg(NO3)2 .6H2O and
NaOH, of the present invention is to utilize hydro-thermal method（The h of crystallization 48 under the conditions of 160 DEG C）The class montmorillonite of synthesis.
Montmorillonite is the natural stratiform mineral matter of a class rich reserves, oxygen or hydroxyl that its structure is not shared between layers
Base, is combined by electrostatic attraction by cation between laminate, and adhesion is weaker, and laminate is easily peeled off.
The content of the invention
The spy that veneer structure after peeling off and peeling off is capable of stable existence is easily achieved based on above-mentioned class montmorillonite or montmorillonite
Point, the present invention provides a kind of inorganic supermolecule electric double layer two-dimensional nano piece, by the moon more from montmorillonite or class montmorillonite
The anions and canons conjugate similar to inorganic salts that the two-dimensional nano lamella of ion is formed with cation by electrostatic interaction, i.e.,
Crystalline state nanoscale twins combine one layer of counter ion counterionsl gegenions of oppositely charged per se with a kind of electric charge, sheet surfaces by electrostatic attraction
The electric double layer two-dimensional nano piece of formation.
In a preferred embodiment of the present invention, the crystalline state nanoscale twins refer to the negatively charged of montmorillonite or class montmorillonite
The laminate of lotus, described counter ion counterionsl gegenions are one or more in hydrogen ion, lithium ion, sodium ion, potassium ion, rubidium ion.
Another aspect of the present invention also provides the preparation method of above-mentioned inorganic supermolecule electric double layer two-dimensional nano piece, covers de- with class
Soil layer plate is matrix, is comprised the following steps：Class montmorillonite is mixed with water, 1-40 g.L are prepared-1Suspension, at 25-55 DEG C
5-10 h are stirred in water-bath, the stripper of class montmorillonite is obtained, then to added in stripper a certain amount of acid or containing lithium ion,
Sodium ion, potassium ion, the salting liquid of rubidium ion, obtain flocculent deposit, then carry out suction filtration, and institute is can't detect in washing to filtrate
After acid radical anion, drying obtains the inorganic supermolecule electric double layer two-dimensional nano piece.
Another aspect of the present invention also provides another preparation method of above-mentioned inorganic supermolecule electric double layer two-dimensional nano piece, with
Montmorillonite laminate is matrix, is comprised the following steps：First montmorillonite is obtained using wet purification, sodium treatment, acid treatment successively
Acid montmorillonite, the acid montmorillonite that will be obtained, water, TBAH mix according to certain ratio, stir at room temperature
Mix 1-10 days, obtain colloidal solution, to adding a certain amount of inorganic acid in the solution or containing lithium ion, sodium ion, potassium ion, rubidium
The salting liquid of ion, obtains flocculent deposit, then carries out suction filtration, washing, and drying obtains the inorganic supermolecule electric double layer two dimension
Nanometer sheet.
In a preferred embodiment of the present invention, the inorganic acid described in above-mentioned preparation method is hydrochloric acid, nitric acid or sulfuric acid
In one or more, the mass fraction of inorganic acid or salt is 1.1wt%-30wt%, and addition is 10-40 ml.
In a preferred embodiment of the present invention, described wet purification, sodium treatment refer to by mass fraction be 5 ~
After 25% montmorillonite solution is stirred at room temperature a period of time, the sodium carbonate liquor that mass fraction is 1 ~ 10% is added thereto to,
1-5 h are stirred in 40-90 DEG C of water-bath, suction filtration, washing is dried to obtain sodium montmorillonite.
In a preferred embodiment of the present invention, described acid treatment refers to that the sodium montmorillonite that will be obtained is molten with inorganic acid
Liquid stirs 24-72 h in 60-95 DEG C of water-bath, and suction filtration, washing is dried to obtain acid montmorillonite.
In a preferred embodiment of the present invention, acid montmorillonite and the mass ratio of water are 0.05-2:1800, the four of addition
Butyl ammonium hydroxide makes the pH of solution between 8.5-10.5.
In a preferred embodiment of the present invention, described drying is that 2-12 h are dried at 100-130 DEG C.
Compared with prior art, the montmorillonite of present invention preparation, the inorganic supermolecule electric double layer nanometer sheet of class montmorillonite base are
The double electricity constituted similar to inorganic salts that a kind of sheet polyanionic nanometer chip is formed with multiple cations by electrostatic interaction
Layer supramolecular materials.The material has broad application prospects, such as can be as inorganic ion exchanger, as solid super-strong acid etc.
Sewage disposal and catalyst field are applied to, the additive of anticorrosive paint can also be applied to significantly improve the anticorrosion of coating
Performance.
Brief description of the drawings
The X-ray powder diffraction figure of sample in Fig. 1 embodiments 1,2,3；
The SEM figures of sample in Fig. 2 embodiments 1；
The HRTEM figures of sample in Fig. 3 embodiments 1.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, but
It is that should be appreciated that these descriptions simply further illustrate the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
Embodiment 1：
Weigh 0.60 g class montmorillonites to be put into beaker, add 30 ml deionized waters, 5 are stirred in 25 DEG C of water-baths
H, obtains transparent homogeneous colloidal solution.Make colloidal coagulation to the hydrochloric acid solution that 15 ml 1.1wt% are added dropwise in the colloidal solution
Afterwards, suction filtration, washing is dried to obtain sample, and the x-ray diffractogram of powder spectrum of gained sample is shown in Fig. 1 .a.The SEM figures of gained sample
As shown in Figure 2.The high-resolution-ration transmission electric-lens figure of gained sample is as shown in Figure 3.
Embodiment 2：
0.90 g class montmorillonites are weighed, 30ml deionized waters are added, 5 h are stirred in 25 DEG C of water-baths, obtain transparent equal
One colloidal solution.To being added dropwise in the colloidal solution after the hydrochloric acid solution of 15 ml 1.1wt% makes colloidal coagulation, suction filtration, washing,
It is dried to obtain sample.The x-ray diffractogram of powder spectrum of gained sample is shown in Fig. 1 .b.
Embodiment 3：
0.90 g class montmorillonites are weighed, 30 ml deionized waters are added, 5 h are stirred in 45 DEG C of water-baths, obtain transparent
Homogeneous colloidal solution.After making colloidal coagulation to the hydrochloric acid solution for adding 15 ml 1.1wt% in the colloidal solution, suction filtration is washed
Wash, be dried to obtain sample.
Embodiment 4：
Weigh 15 g montmorillonites to be put into there-necked flask, add 85 ml deionized waters to stir at room temperature, add 0.6 g
Solid Na2CO3, 1 h is stirred in 60 DEG C of water-baths, suction filtration, washing is dried to obtain sodium montmorillonite.Take 3.0 g sodiums illiteracy
De- soil is put into beaker, adds 200 ml 1.1wt% hydrochloric acid solutions, is put in 90 DEG C of h of stirred in water bath 24, and suction filtration, washing is done
It is dry to obtain acid montmorillonite.Take 1.0 g sodiums montmorillonites to be mixed in beaker with 100 ml deionized waters, four fourths of a few drops are added dropwise
Base ammonium hydroxide is vigorously mixed at room temperature for obtaining montmorillonite stripper in one week or so to the pH=10 or so of solution（Colloid is molten
Liquid）.After making colloidal coagulation to the hydrochloric acid solution for adding 30 ml 1.1wt% in the stripper, suction filtration, washing is dried to obtain sample
Product.
Embodiment 5：
Weigh 15 g montmorillonites to be put into there-necked flask, add 85 ml deionized waters to stir at room temperature, add 0.6 g
Solid Na2CO3, 1 h is stirred in 60 DEG C of water-baths, suction filtration, washing is dried to obtain sodium montmorillonite.Take 3.0 g sodiums illiteracy
De- soil is put into beaker, adds 200 ml 1.1wt% hydrochloric acid solutions, is put in 90 DEG C of h of stirred in water bath 24, and suction filtration, washing is done
It is dry to obtain acid montmorillonite.Take 1.0 g sodiums montmorillonites to be mixed in beaker with 100 ml deionized waters, four fourths of a few drops are added dropwise
Base ammonium hydroxide is vigorously mixed at room temperature for obtaining montmorillonite stripper in one week or so to the pH=10 or so of solution.To the stripping
The NaCl solution of 30 ml 5wt% is added in liquid, makes suction filtration after colloidal coagulation, washed, be dried to obtain sample.The powder of gained sample
Last X ray diffracting spectrum is shown in Fig. 1 .c.
Above example has been shown and described general principle of the invention and principal character and advantages of the present invention.The industry
Technical staff it should be appreciated that the present invention is not limited to the above embodiments, described in above-described embodiment and specification simply
Principle of the invention is illustrated, rather than the scope of the present invention is limited by any way, without departing from the scope of the invention,
Various changes and modifications of the present invention are possible, and these changes and improvements are both fallen within claimed scope.
Claims (6)
1. a kind of inorganic supermolecule electric double layer two-dimensional nano piece, it is characterised in that be prepared via a method which to obtain：With montmorillonite
Laminate is matrix, is comprised the following steps：First montmorillonite is obtained acidifying and covered using wet purification, sodium treatment, acid treatment successively
De- soil, the acid montmorillonite that will be obtained, water, TBAH mix according to certain ratio, and 1-10 is stirred at room temperature
My god, colloidal solution is obtained, to adding a certain amount of inorganic acid in the solution or containing lithium ion, sodium ion, potassium ion, rubidium ion
Salting liquid, obtains flocculent deposit, then carries out suction filtration, and washing, drying obtains the inorganic supermolecule electric double layer two-dimensional nano piece.
2. the inorganic supermolecule electric double layer two-dimensional nano piece described in claim 1, it is characterised in that inorganic acid described above is
One or more in hydrochloric acid, nitric acid or sulfuric acid, the mass fraction of inorganic acid or salting liquid is 1.1wt%-30wt%, and addition is
10-40 ml。
3. the preparation method of the inorganic supermolecule electric double layer two-dimensional nano piece described in claim 1, it is characterised in that described is wet
After method purification, sodium treatment refer to for the montmorillonite solution that mass fraction is 5 ~ 25% a period of time being stirred at room temperature, Xiang Qi
It is middle to add the sodium carbonate liquor that mass fraction is 1 ~ 10%, 1-5 h are stirred in 40-90 DEG C of water-bath, suction filtration, washing is dried
Obtain sodium montmorillonite.
4. the preparation method of the inorganic supermolecule electric double layer two-dimensional nano piece described in claim 1, it is characterised in that described acid
Treatment refers to that the sodium montmorillonite that will be obtained stirs 24-72 h with inorganic acid solution in 60-95 DEG C of water-bath, and suction filtration is washed
Wash, be dried to obtain acid montmorillonite.
5. the preparation method of the inorganic supermolecule electric double layer two-dimensional nano piece described in claim 1, it is characterised in that acidifying is covered de-
Soil is 0.05-2 with the mass ratio of water:1800, the TBAH of addition makes the pH of solution between 8.5-10.5.
6. the preparation method of the inorganic supermolecule electric double layer two-dimensional nano piece described in claim 1, it is characterised in that the drying
It is that 2-12 h are dried at 100-130 DEG C.
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| CN105860618B (en) * | 2016-05-26 | 2018-10-30 | 北京化工大学 | A kind of electric double layer anticorrosive paint and its application |
| CN105964287A (en) * | 2016-06-06 | 2016-09-28 | 北京化工大学 | Inorganic double-electrode-layer solid polyacid and preparation method and application thereof |
| CN110034296B (en) * | 2019-04-19 | 2022-02-15 | 哈尔滨工业大学 | Convex mirror-shaped silicon nanosheet material and preparation method and application thereof |
| CN114085342B (en) * | 2021-12-10 | 2023-12-05 | 安徽陶博士环保科技有限公司 | Photo-cured fiber reinforced double-electric-layer nano ceramic coiled material and preparation method thereof |
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Effective date of registration: 20200113 Address after: 233000 Anhui city in Bengbu Province, Yanshan Road No. 410 Building 1 homes Shanxiang Patentee after: Anhui Dr. Tao Environmental Protection Technology Co., Ltd. Address before: 100029 Beijing, North Third Ring Road, No. 15 East Road, Chaoyang District Patentee before: Beijing University of Chemical Technology |