CN108059182A - A kind of preparation method of rare earth layered hydroxide nanometer sheet and its colloidal sol - Google Patents
A kind of preparation method of rare earth layered hydroxide nanometer sheet and its colloidal sol Download PDFInfo
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- CN108059182A CN108059182A CN201810094116.4A CN201810094116A CN108059182A CN 108059182 A CN108059182 A CN 108059182A CN 201810094116 A CN201810094116 A CN 201810094116A CN 108059182 A CN108059182 A CN 108059182A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/282—Sulfates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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Abstract
A kind of rare earth layered hydroxide nanometer sheet of the present invention and its preparation method of colloidal sol, nanometer sheet preparation comprise the following steps：The lanthanum nitrate hexahydrate of respective concentration is configured to, ammonium sulfate is dissolved in lanthanum nitrate hexahydrate by proportioning, forms mixed liquor, pH of mixed is adjusted to 6~10, and uniform suspension is persistently stirred to get, reaction obtains product, centrifuges and be dried to obtain immediately rare earth layered hydroxide La2(OH)4SO4·nH2O nanometer sheets.And by proportioning, the nanometer sheet prepared is placed in formamide solution after ultrasonic centrifugal treating, takes upper liquid, relevant nanometer film sol is made.The application using ice bath method reduce activation can a step prepare rare earth layered hydroxide La2(OH)4SO4·nH2O nanometer sheets, the method that solving the problems, such as such compound in the prior art can not use traditional intercalation to remove prepare individual layer nanometer sheet, and simple for process, easy to operate, can mass production, relevant nanometer film sol stability is good, saves raw material.
Description
Technical field：
The invention belongs to materials science fields, and in particular to a kind of rare earth layered hydroxide nanometer sheet and its colloidal sol
Preparation method.
Background technology：
La2(OH)4SO4·nH2O is rare earth lamellar compound RE2(OH)4SO4·nH2One kind in O.Belong to anionic
Lamellar compound, hydroxide main stor(e)y plate is by nine coordination polyhedrom [LaO9] be formed by connecting by coplanar and public security frontier bureau, interlayer
SO4 2-Tetrahedron then plays charge balanced action with adjacent two main stor(e)ies plate Covalent bonding together respectively by two nonadjacent oxygen atoms.The change
It closes object and does not possess traditional rare earth lamellar compound (such as RE2(OH)5A·nH2O, A=Cl, NO3Deng) ion-exchange performance, therefore
Can not ultrathin nanometer piece be prepared by the process route of pillared-stripping.The advantages of it is notable is its special stoicheiometry：The change
Close the La/S molar ratios of object and the oxygen-containing lanthanum sulfate (La of rare earth2O2SO4) and sulphur lanthana (La2O2S it is) completely the same, therefore can conduct
Prepare the preferable presoma of the two classes compound.It is existing to study the advantage for also demonstrating the route really：In this kind of stratiform chemical combination
It is sulphur source that mild ammonium sulfate is used in the building-up process of object, and calcines and prepare La2O2SO4And La2O2By-product is only during S
For vapor.The use containing sulfur feedstock for successfully overcoming that tradition prepares that environment in rare-earth oxide sulfate method is harmful to or ring
The problem of discharge for the product that border is harmful to.Oxygen-containing lanthanum sulfate (the La of rare earth2O2SO4) and sulphur lanthana (La2O2S) in numerous areas
There is good application value, and the character of the character pair product of presoma has tremendous influence.Therefore to La2(OH)4SO4·
nH2The research of O synthesis is most important, has on the existing research of the compound：Researcher Sasaki in 2010 etc. is with rare earth
Sulfate and four ammonium of hexa-methylene are raw material, synthesize this kind of sulfate type lamellar compound RE for the first time using sluggish precipitation2
(OH)4SO4·nH2O (RE=Pr-Tb, n~2).But because different rare earth element properties are different, this report is only reported using precipitation
Method prepares such compound of RE=Pr-Tb.La2(OH)4SO4·nH2The report of O is seen 2013 earliest, has researcher to adopt
This kind of compound has been prepared with hydro-thermal method.2014 Nian You researchers use the precipitation method to obtain La by precipitating reagent of ammonium hydroxide2
(OH)4SO4·nH2O.In conclusion La is prepared at present2(OH)4SO4·nH2The method of O is only limitted to hydro-thermal method and the precipitation method.Mesh
Before there are the problem of be：1) in terms of synthetic technology route, such as hexa of precipitating reagent used in the precipitation method has at room temperature
Hydrolyze the shortcomings of easily generating formaldehyde and its derivative under slow, high temperature in air and reduce precipitation reaction yield.Though hydro-thermal method
The disadvantages mentioned above of the precipitation method is so overcome, and there are the advantages such as product purity is high, pollution is small, but reaction process needs under hydrothermal condition
Large energy is wanted, and the stability of reaction process is poor.2) in gained target product properties：Hydro-thermal method and the room temperature precipitation method
Prepared La2(OH)4SO4·nH2O is especially precipitated because the higher final crystallization of reaction temperature is thicker nanometer or micron film
There is largely agglomeration in method products therefrom, dispersiveness is poor.The pattern of presoma will significantly affect its corresponding calcining
The pattern of product, thus the La using this thick lamellar compound obtained by presoma2O2SO4And La2O2S is also larger
Grain.And both approaches are all difficult to realize be prepared on a large scale.In addition, the laminate thickness of the nanometer sheet prepared using both approaches
Degree is up to 30~300nm, and because this kind of compound can not prepare nanometer sheet through intercalation-stripping and therefore can not obtain at present
Well-crystallized and thickness only several nanometers of ultra-thin rare earth layered hydroxide La2(OH)4SO4·nH2O nanometer sheets, therefore can not
Obtain the rare earth layered hydroxide La having good stability2(OH)4SO4·nH2O nano-film sols.
The content of the invention：
The purpose of the present invention is be directed to rare earth layered hydroxide La2(OH)4SO4·nH2O nanometer sheets and its colloidal sol are existing
Problem present in preparation process provides a kind of rare earth layered hydroxide La2(OH)4SO4·nH2O nanometer sheets and its colloidal sol
Preparation method.
To achieve the above object, the present invention uses following technical scheme：
A kind of rare earth layered hydroxide La2(OH)4SO4·nH2The preparation method of O nanometer sheets, comprises the following steps：
(1) by lanthanum nitrate hexahydrate (La (NO3)3·6H2O) it is uniformly mixed in deionized water, is configured to lanthanum nitrate (La
(NO3)3) solution, wherein, the lanthanum nitrate (La (NO3)3) solution La3+Concentration is 0.03~0.20mol/L；
(2) by ammonium sulfate ((NH4)2SO4) it is dissolved in lanthanum nitrate (La (NO3)3) in solution, mixed liquor is formed, wherein,
The ammonium sulfate ((NH4)2SO4) and lanthanum nitrate (La (NO3)3) solution addition in molar ratio, SO4 2-：La3+=
0.5~10；
(3) ammonium hydroxide is added in into mixed liquor, adjusts pH of mixed to 6~10, and continues to stir, obtains uniform suspension；
(4) uniform suspension is reacted, obtains product；Wherein, the reaction temperature is -4~4 DEG C, during reaction
Between be 1~48h；
(5) it is immediately centrifuged after reaction, rare earth layered hydroxide La is dried to obtain after centrifugation2
(OH)4SO4·nH2O nanometer sheets, wherein, the drying temperature is 30~70 DEG C, drying time for 12~for 24 hours, n=1.5~
2.5。
A kind of rare earth layered hydroxide La2(OH)4SO4·nH2The preparation method of O nano-film sols, by above-mentioned preparation
Rare earth layered hydroxide La2(OH)4SO4·nH2O nanometer sheets are prepared, and comprise the following steps：
(1) by proportioning, the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometers of tablet qualities：Formamide solution
Volume=0.1：(100~300), unit g:Ml takes the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometer sheets,
It is placed in formamide solution；
(2) rare earth layered hydroxide La will be contained2(OH)4SO4·nH2The formamides of O nanometer sheets it is molten through ultrasonic centrifugation at
After reason, upper liquid is taken, rare earth layered hydroxide La is made2(OH)4SO4·nH2O nano-film sols.
The rare earth layered hydroxide La2(OH)4SO4·nH2In O nanometers of piece preparation methods, the step (2)
In, by ammonium sulfate ((NH4)2SO4) in lanthanum nitrate (La (NO3)3) dissolution time in solution is 10~20min, it is dissolved to
Clarification completely.
The rare earth layered hydroxide La2(OH)4SO4·nH2In O nanometers of piece preparation methods, the step (3)
In, the mixing time for forming uniform suspension is 10~30min.
The rare earth layered hydroxide La2(OH)4SO4·nH2In O nanometers of piece preparation methods, the step (4)
In, product component is the rare earth layered hydroxide La containing the mother liquor not reacted completely with absorption water2(OH)4SO4·nH2O receives
Rice piece.
The rare earth layered hydroxide La2(OH)4SO4·nH2In O nanometers of piece preparation methods, the step (5)
In, the revolution of centrifugation is 9000~12000r/min, and the time is 10~20min.
The rare earth layered hydroxide La2(OH)4SO4·nH2In O nanometers of piece preparation methods, the step (5)
In, the nanometer sheet thickness of preparation is 3~8nm.
The rare earth layered hydroxide La2(OH)4SO4·nH2In O nano-film sol preparation methods, the step
(2) in, ultrasonic time is 20~50min, and centrifugal rotational speed is 8000~12000r/min, and centrifugation time is 5~10min, described
Centrifugally operated carried out in centrifuge.
Ice bath method using low temperature reduce lamellar compound activation energy, can not only a step prepare ultrathin nanometer piece, and
Lamellar compound can be produced in enormous quantities.Method is simple, and condition is not harsh.
The principle of the invention is：La2(OH)4SO4·nH2The layer structure of O is regarded as by elementary cell nanometer sheet along a-
Direction of principal axis stacking forms, and this stacking needs higher activation energy.Ice bath method makes full use of low temperature that can not provide enough activation
Can the characteristics of, inhibit the growth of lamellar compound through-thickness, that is, prevent laminate along a- direction of principal axis stacking, so as to which a step obtains ruler
Very little controllable ultra-thin La2(OH)4SO4·nH2O nanometer sheets.
Beneficial effects of the present invention：
(1) the application using ice bath method reduce activation can a step prepare ultra-thin rare earth layered hydroxide La2(OH)4SO4·nH2O nanometer sheets, solve in the prior art such compound because interlayer sulfate ion and main stor(e)y plate pass through covalent bond
It connects and the method for traditional intercalation-stripping can not be used to prepare the problem of individual layer nanometer sheet；
(2) the rare earth layered hydroxide La of the application is used2(OH)4SO4·nH2It is prepared by the preparation method of O nanometer sheets
It is simple for process, it is easy to operate, it can the ultra-thin rare earth layered hydroxide La of mass production2(OH)4SO4·nH2O nanometer sheets；
(3) the ultrathin nanometer piece prepared using low temperature ice bath method prepares relevant nanometer film sol as raw material, and stability is good, saves
Raw material.
Description of the drawings：
Fig. 1 is rare earth layered hydroxide La prepared by the embodiment of the present invention 12(OH)4SO4·nH2The XRD diagram of O nanometer sheets
Spectrum；
Fig. 2 is rare earth layered hydroxide La prepared by the embodiment of the present invention 32(OH)4SO4·nH2The XRD diagram of O nanometer sheets
Spectrum；
Fig. 3 is rare earth layered hydroxide La prepared by the embodiment of the present invention 52(OH)4SO4·nH2The XRD diagram of O nanometer sheets
Spectrum.
Specific embodiment：
With reference to embodiment, the present invention is described in further detail.
In following embodiment：
Lanthanum nitrate hexahydrate (La (NO3)3·6H2O), the raw materials such as ammonium sulfate and formamide solution are all from purchased in market, first
Amide solution is pure to analyze.
Embodiment 1
A kind of rare earth layered hydroxide La2(OH)4SO4·nH2The preparation method of O nanometer sheets, which is characterized in that including
Following steps：
(1) by lanthanum nitrate hexahydrate (La (NO3)3·6H2O) it is uniformly mixed in deionized water, is configured to La3+Concentration is
Lanthanum nitrate (La (the NO of 0.03mol/L3)3) solution；
(2) addition in molar ratio, SO4 2-：La3+=0.5, by ammonium sulfate ((NH4)2SO4) it is dissolved in lanthanum nitrate (La
(NO3)3) in solution, 10min is dissolved, complete clarification is dissolved to, forms mixed liquor；
(3) ammonium hydroxide is added in into mixed liquor, adjusts pH of mixed to 6, and continues to stir 10min, obtains uniform suspension；
(4) uniform suspension is reacted, reaction temperature is 4 DEG C, reaction time 48h, obtains product, product component
For the rare earth layered hydroxide La for containing the mother liquor not reacted completely with adsorbing water2(OH)4SO4·nH2O nanometer sheets；
(5) it is immediately centrifuged after reaction, the revolution of centrifugation is 9000r/min, time 20min,
After centrifugation, at 30 DEG C, drying for 24 hours, obtains rare earth layered hydroxide La2(OH)4SO4·nH2O nanometer sheets, thickness are
6~8nm, n=1.5, the shape hydroxide La2(OH)4SO4·nH2O nanometer sheet XRD spectrums are as shown in Figure 1.
Using the rare earth layered hydroxide La of above-mentioned preparation2(OH)4SO4·nH2O nanometer sheets, rare earth layered hydroxide
La2(OH)4SO4·nH2O nano-film sols, specifically include following steps：
(1) by proportioning, the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometers of tablet qualities：Formamide solution
Volume=0.1：100, unit g:Ml takes the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometer sheets, are placed in first
In amide solution；
(2) rare earth layered hydroxide La will be contained2(OH)4SO4·nH2The formamide of O nanometer sheets is molten through ultrasonic 20min
After processing, the centrifugal treating in centrifuge, centrifugal rotational speed 8000r/min, centrifugation time 10min take upper liquid, the upper strata
Liquid is rare earth layered hydroxide La obtained2(OH)4SO4·nH2O nano-film sols can be stabilized 10 days.
Embodiment 2
A kind of rare earth layered hydroxide La2(OH)4SO4·nH2The preparation method of O nanometer sheets, which is characterized in that including
Following steps：
(1) by lanthanum nitrate hexahydrate (La (NO3)3·6H2O) it is uniformly mixed in deionized water, is configured to La3+Concentration is
Lanthanum nitrate (La (the NO of 0.20mol/L3)3) solution；
(2) addition in molar ratio, SO4 2-：La3+=10, by ammonium sulfate ((NH4)2SO4) it is dissolved in lanthanum nitrate (La
(NO3)3) in solution, 20min is dissolved, complete clarification is dissolved to, forms mixed liquor；
(3) ammonium hydroxide is added in into mixed liquor, adjusts pH of mixed to 10, and continues to stir 30min, is obtained uniformly suspended
Liquid；
(4) uniform suspension is reacted, reaction temperature is 0 DEG C, reaction time 1h, obtains product, product component
For the rare earth layered hydroxide La for containing the mother liquor not reacted completely with adsorbing water2(OH)4SO4·nH2O nanometer sheets；
(5) it is immediately centrifuged after reaction, the revolution of centrifugation is 12000r/min, time 10min,
After centrifugation, at 50 DEG C, dry 22h obtains rare earth layered hydroxide La2(OH)4SO4·nH2O nanometer sheets, thickness are
5~7nm, n=2.5.
Using the rare earth layered hydroxide La of above-mentioned preparation2(OH)4SO4·nH2O nanometer sheets, rare earth layered hydroxide
La2(OH)4SO4·nH2O nano-film sols, specifically include following steps：
(1) by proportioning, the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometers of tablet qualities：Formamide solution
Volume=0.1:300, unit g:Ml takes the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometer sheets, are placed in first
In amide solution；
(2) rare earth layered hydroxide La will be contained2(OH)4SO4·nH2The formamide of O nanometer sheets is molten through ultrasonic 50min
After processing, the centrifugal treating in centrifuge, centrifugal rotational speed 12000r/min, centrifugation time 5min take upper liquid, are made dilute
Native layered hydroxide La2(OH)4SO4·nH2O nano-film sols can be stabilized 20 days.
Embodiment 3
A kind of rare earth layered hydroxide La2(OH)4SO4·nH2The preparation method of O nanometer sheets, which is characterized in that including
Following steps：
(1) by lanthanum nitrate hexahydrate (La (NO3)3·6H2O) it is uniformly mixed in deionized water, is configured to La3+Concentration is
Lanthanum nitrate (La (the NO of 0.1mol/L3)3) solution；
(2) addition in molar ratio, SO4 2-：La3+=3, by ammonium sulfate ((NH4)2SO4) it is dissolved in lanthanum nitrate (La
(NO3)3) in solution, 14min is dissolved, complete clarification is dissolved to, forms mixed liquor；
(3) ammonium hydroxide is added in into mixed liquor, adjusts pH of mixed to 9, and continues to stir 20min, obtains uniform suspension；
(4) uniform suspension is reacted, reaction temperature is -4 DEG C, and the reaction time for for 24 hours, obtains product, product into
It is divided into the rare earth layered hydroxide La containing the mother liquor not reacted completely with absorption water2(OH)4SO4·nH2O nanometer sheets；
(5) it is immediately centrifuged after reaction, the revolution of centrifugation is 9000r/min, time 20min,
After centrifugation, at 40 DEG C, dry 18h obtains rare earth layered hydroxide La2(OH)4SO4·nH2O nanometer sheets, thickness are
3~5nm, n=2.0, the shape hydroxide La2(OH)4SO4·nH2O nanometer sheet XRD spectrums are as shown in Figure 2.
Using the rare earth layered hydroxide La of above-mentioned preparation2(OH)4SO4·nH2O nanometer sheets, rare earth layered hydroxide
La2(OH)4SO4·nH2O nano-film sols, specifically include following steps：
(1) by proportioning, the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometers of tablet qualities：Formamide solution
Volume=0.1：150, unit g:Ml takes the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometer sheets, are placed in first
In amide solution；
(2) rare earth layered hydroxide La will be contained2(OH)4SO4·nH2The formamide of O nanometer sheets is molten through ultrasonic 30min
After processing, the centrifugal treating in centrifuge, centrifugal rotational speed 9000r/min, centrifugation time 8min take upper liquid, are made dilute
Native layered hydroxide La2(OH)4SO4·nH2O nano-film sols can be stabilized 12 days.
Embodiment 4
A kind of rare earth layered hydroxide La2(OH)4SO4·nH2The preparation method of O nanometer sheets, which is characterized in that including
Following steps：
(1) by lanthanum nitrate hexahydrate (La (NO3)3·6H2O) it is uniformly mixed in deionized water, is configured to La3+Concentration is
Lanthanum nitrate (La (the NO of 0.15mol/L3)3) solution；
(2) addition in molar ratio, SO4 2-：La3+=4, by ammonium sulfate ((NH4)2SO4) it is dissolved in lanthanum nitrate (La
(NO3)3) in solution, 18min is dissolved, complete clarification is dissolved to, forms mixed liquor；
(3) ammonium hydroxide is added in into mixed liquor, adjusts pH of mixed to 8, and continues to stir 25min, obtains uniform suspension；
(4) uniform suspension is reacted, reaction temperature is 2 DEG C, reaction time 36h, obtains product, product component
For the rare earth layered hydroxide La for containing the mother liquor not reacted completely with adsorbing water2(OH)4SO4·nH2O nanometer sheets；
(5) it is immediately centrifuged after reaction, the revolution of centrifugation is 9500r/min, time 18min,
After centrifugation, at 60 DEG C, drying for 24 hours, obtains rare earth layered hydroxide La2(OH)4SO4·nH2O nanometer sheets, thickness are
5~7nm, n=1.8.
Using the rare earth layered hydroxide La of above-mentioned preparation2(OH)4SO4·nH2O nanometer sheets, rare earth layered hydroxide
La2(OH)4SO4·nH2O nano-film sols, specifically include following steps：
(1) by proportioning, the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometers of tablet qualities：Formamide solution
Volume=0.1：200, unit g:Ml takes the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometer sheets, are placed in first
In amide solution；
(2) rare earth layered hydroxide La will be contained2(OH)4SO4·nH2The formamide of O nanometer sheets is molten through ultrasonic 40min
After processing, the centrifugal treating in centrifuge, centrifugal rotational speed 10000r/min, centrifugation time 80min take upper liquid, are made
Rare earth layered hydroxide La2(OH)4SO4·nH2O nano-film sols are stabilized 15 days.
Embodiment 5
A kind of rare earth layered hydroxide La2(OH)4SO4·nH2The preparation method of O nanometer sheets, which is characterized in that including
Following steps：
(1) by lanthanum nitrate hexahydrate (La (NO3)3·6H2O) it is uniformly mixed in deionized water, is configured to La3+Concentration is
Lanthanum nitrate (La (the NO of 0.20mol/L3)3) solution；
(2) addition in molar ratio, SO4 2-：La3+=6, by ammonium sulfate ((NH4)2SO4) it is dissolved in lanthanum nitrate (La
(NO3)3) in solution, 20min is dissolved, complete clarification is dissolved to, forms mixed liquor；
(3) ammonium hydroxide is added in into mixed liquor, adjusts pH of mixed to 10, and continues to stir 20min, is obtained uniformly suspended
Liquid；
(4) uniform suspension is reacted, reaction temperature be -2 DEG C, reaction time 12h, obtain product, product into
It is divided into the rare earth layered hydroxide La containing the mother liquor not reacted completely with absorption water2(OH)4SO4·nH2O nanometer sheets；
(5) it is immediately centrifuged after reaction, the revolution of centrifugation is 10000r/min, time 15min,
After centrifugation, at 70 DEG C, dry 12h obtains rare earth layered hydroxide La2(OH)4SO4·nH2O nanometer sheets, thickness are
4~6nm, n=2.0, the shape hydroxide La2(OH)4SO4·nH2O nanometer sheet XRD spectrums are as shown in Figure 3.
Using the rare earth layered hydroxide La of above-mentioned preparation2(OH)4SO4·nH2O nanometer sheets, rare earth layered hydroxide
La2(OH)4SO4·nH2O nano-film sols, specifically include following steps：
(1) by proportioning, the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometers of tablet qualities：Formamide solution
Volume=0.1：250, unit g:Ml takes the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometer sheets, are placed in first
In amide solution；
(2) rare earth layered hydroxide La will be contained2(OH)4SO4·nH2The formamide of O nanometer sheets is molten through ultrasonic 40min
After processing, the centrifugal treating in centrifuge, centrifugal rotational speed 11000r/min, centrifugation time 10min take upper liquid, are made
Rare earth layered hydroxide La2(OH)4SO4·nH2O nano-film sols are stabilized 18 days.
Claims (7)
1. a kind of rare earth layered hydroxide La2(OH)45O4·nH2The preparation method of O nanometer sheets, which is characterized in that including following
Step：
(1) by lanthanum nitrate hexahydrate (La (NO3)3·6H2O) it is uniformly mixed in deionized water, is configured to lanthanum nitrate (La (NO3)3)
Solution, wherein, the lanthanum nitrate (La (NO3)3) solution La3+Concentration is 0.03~0.20mol/L；
(2) by ammonium sulfate ((NH4)2SO4) it is dissolved in lanthanum nitrate (La (NO3)3) in solution, mixed liquor is formed, wherein, it is described
Ammonium sulfate ((NH4)2SO4) and lanthanum nitrate (La (NO3)3) solution addition in molar ratio, 5O4 2-∶La3+=0.5~
10；
(3) ammonium hydroxide is added in into mixed liquor, adjusts pH of mixed to 6~10, and continues to stir, obtains uniform suspension；
(4) uniform suspension is reacted, obtains product；Wherein, the reaction temperature is -4~4 DEG C, the reaction time 1
~48h；
(5) it is immediately centrifuged after reaction, rare earth layered hydroxide La is dried to obtain after centrifugation2(OH)4SO4·nH2O nanometer sheets, wherein, the drying temperature is 30~70 DEG C, drying time for 12~for 24 hours, n=1.5~2.5.
2. rare earth layered hydroxide La according to claim 12(OH)4SO4·nH2The preparation method of O nanometer sheets, it is special
Sign is, in the step (2), by ammonium sulfate ((NH4)2SO4) in lanthanum nitrate (La (NO3)3) dissolving in solution when
Between be 10~20min.
3. rare earth layered hydroxide La according to claim 12(OH)4SO4·nH2The preparation method of O nanometer sheets, it is special
Sign is, in the step (3), the mixing time for forming uniform suspension is 10~30min.
4. rare earth layered hydroxide La according to claim 12(OH)45O4·nH2The preparation method of O nanometer sheets, it is special
Sign is, in the step (5), the revolution of centrifugation is 9000~12000r/min, and the time is 10~20min.
5. rare earth layered hydroxide La according to claim 12(OH)4SO4·nH2The preparation method of O nanometer sheets, it is special
Sign is, in the step (5), the nanometer sheet thickness of preparation is 3~8nm.
6. a kind of rare earth layered hydroxide La2(OH)4SO4·nH2O nano-film sol preparation methods, which is characterized in that described
Rare earth layered hydroxide La2(OH)45O4·nH2The rare earth layered hydroxide La that O nano-film sols are prepared by claim 12
(OH)4SO4·nH2O nanometer sheets are prepared, and specifically include following steps：
(1) by proportioning, the rare earth layered hydroxide La of preparation2(OH)4SO4·nH2O nanometers of tablet qualities: formamide solution volume
=0.1: (100~300), unit g：Ml, the rare earth layered hydroxide La that claim 1 is taken to prepare2(OH)4SO4·nH2O receives
Rice piece, is placed in formamide solution；
(2) rare earth layered hydroxide La will be contained2(OH)4SO4·nH2The formamide of O nanometer sheets is molten after ultrasonic centrifugal treating,
Upper liquid is taken, rare earth layered hydroxide La is made2(OH)4SO4·nH2O nano-film sols.
7. rare earth layered hydroxide La according to claim 62(OH)4SO4·nH2O nano-film sol preparation methods,
It is characterized in that, in the step (2), ultrasonic time is 20~50min, and centrifugal rotational speed is 8000~12000r/min, is centrifuged
Time is 5~10min.
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| CN109135744A (en) * | 2018-05-30 | 2019-01-04 | 渤海大学 | A kind of novel tungstates NaLaW2O7(OH)2(H2O) and preparation method thereof |
| CN109665561A (en) * | 2019-02-01 | 2019-04-23 | 渤海大学 | A kind of REVO4From sacrifice method for preparing template |
| CN109694046A (en) * | 2019-02-01 | 2019-04-30 | 渤海大学 | A method of rare earth orthophosphates is prepared using from sacrifice template |
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| CN108298600A (en) * | 2018-04-13 | 2018-07-20 | 厦门大学 | A kind of environment-friendly preparation method thereof of two dimension hydroxide nano piece |
| CN109135744A (en) * | 2018-05-30 | 2019-01-04 | 渤海大学 | A kind of novel tungstates NaLaW2O7(OH)2(H2O) and preparation method thereof |
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| CN109694046A (en) * | 2019-02-01 | 2019-04-30 | 渤海大学 | A method of rare earth orthophosphates is prepared using from sacrifice template |
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