CN107098374B - Evenly dispersed bulk morphologies carbonic acid cerium crystal and preparation method thereof - Google Patents
Evenly dispersed bulk morphologies carbonic acid cerium crystal and preparation method thereof Download PDFInfo
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- CN107098374B CN107098374B CN201710381052.1A CN201710381052A CN107098374B CN 107098374 B CN107098374 B CN 107098374B CN 201710381052 A CN201710381052 A CN 201710381052A CN 107098374 B CN107098374 B CN 107098374B
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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
- C01F17/247—Carbonates
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The present invention relates to a kind of preparation methods of blocky carbonic acid cerium crystal, it is in simulation biomineralization environmental system, using disodium ethylene diamine tetraacetate for soft template, soluble cerium salt is raw material, soluble carbonate salt is precipitating reagent, it by mixing, is aged, is filtered, washed and baking step, the carbonic acid cerium crystal of evenly dispersed bulk morphologies is prepared.The present invention utilizes the space complexing power of disodium ethylene diamine tetraacetate, complementary by Lattice Matching and spatial chemistry, regulates and controls to the nucleation and crystal growth of cerous carbonate, has obtained the carbonic acid cerium crystal of granularity, pattern and structure-controllable；Preparation method has the characteristics that low in raw material price, reaction condition are mild, low energy consumption, is suitble to industrialized production.
Description
Technical field
The present invention relates to powder body material technical fields, and in particular to a kind of evenly dispersed bulk morphologies carbonic acid cerium crystal and
Preparation method.
Background technique
Baotou rare earth is resourceful, and the characteristics of Baotou rare earth resource is occupied an leading position with light rare earth, and wherein cerium contains
Amount accounts for 50%, therefore it is particularly important to develop cerium resources advantage.Cerium oxide has the property of N-type semiconductor, there is unique 4f electronics
Structure shows excellent oxygen storage capacity and charge-exchange ability, is widely used in three-way catalyst, fuel cell, light and urges
The fields such as change, pollutant treatment, glass polishing agent and electronic ceramics.
In recent years, the domestic demand to special appearance cerium oxide is increasingly vigorous, and the application of cerium oxide requires that its particle has
There is special physical property, such as pattern, size, structure, dispersibility, the surface property of particle, these physical and chemical performances determine its application
Therefore it is just very necessary to seek eased controllable preparation method in field.Mineralization method introducing is prepared into special appearance
Cerium oxide, be expected to realize cerium oxide pattern, size distribution and structure effective control.Ceria when due to low-temperature bake
Pattern there is heredity, so the pattern of cerium oxide can be controlled by the cerous carbonate of synthesis special appearance.Template is made
For synthetic material controlling agent, the self assembling process of material is directly taken part in.Currently, having prepared ball using different templates
Shape, rodlike and flower-shaped etc. different-shapes cerium oxide had not been reported as blocky carbonic acid cerium crystal.
Summary of the invention
For the defects in the prior art, it is an object of that present invention to provide a kind of evenly dispersed bulk morphologies cerous carbonate is brilliant
Body and preparation method thereof, with by the complexing and space structure that utilize disodium ethylene diamine tetraacetate, by Lattice Matching and
Stereochemical structure complementation controls cerous carbonate nucleation process and crystal growth, obtains the bulk of particle size uniformity, morphological rules
Shape carbonic acid cerium crystal；Entire reaction process carries out at room temperature, and reaction condition is mild, and method is simple, easily controllable.
To achieve the above object, technical solution provided by the invention are as follows:
In a first aspect, including the following steps: S1 the present invention provides a kind of preparation method of blocky carbonic acid cerium crystal:
Template is added in cerium solution, is uniformly mixed, adjusts pH value to 3~5, obtains mixed liquor；S2: precipitating is added in mixed liquor
The aqueous solution of agent is aged after stirring；S3: the product that ageing obtains successively is filtered, washed and dried, bulk is obtained
Carbonic acid cerium crystal.It should be noted that the process of addition can be with continuous stirring in S1 and S2.
In further embodiment of the invention, in the mixed liquor of S1, Ce3+Molar concentration be 0.05~0.58mol/
L, the concentration of template are 3~12g/L.
In further embodiment of the invention, in S2, the mass ratio of precipitating reagent and cerium salt is 1:(0.5~2), precipitating
The molar concentration of precipitating reagent is 0.04~0.58mol/L in the aqueous solution of agent.
In further embodiment of the invention, in S2, it is incorporated as being slowly added to, time of adition process is 0.5~
4h；The time of stirring is 0.5h.
In further embodiment of the invention, in S2, the time of ageing is 0.5~48h.
In further embodiment of the invention, in S1, cerium salt is water-soluble cerium salt, water-soluble cerium salt packet
Include one of cerous nitrate, cerium chloride, cerous acetate and cerous sulfate or a variety of.
In further embodiment of the invention, in S2, precipitating reagent is soluble carbonate salt, and soluble carbonate salt includes
One of ammonium carbonate, ammonium hydrogen carbonate, sodium carbonate and sodium bicarbonate are a variety of.
In further embodiment of the invention, in S1, template is disodium ethylene diamine tetraacetate.
In further embodiment of the invention, S3 is specifically included: the product that ageing is obtained filters, and collects filter cake；
Filter cake is washed 3 times using deionized water, then alcohol is washed 2 times；Filter cake after alcohol is washed obtains blocky carbonic acid in 60 DEG C of drying 2h
Cerium crystal.
Second aspect, the present invention provides the blocky cerous carbonates that the preparation method using blocky carbonic acid cerium crystal is prepared
Crystal.The present invention be simulation biomineralization liquid-phase precipitation system in, be using disodium ethylene diamine tetraacetate (EDTA-2Na)
Soft template, soluble cerium salt are raw material, and the precipitating reagent containing carbonate is added, and by ageing, filtering, drying, have been prepared
The carbonic acid cerium crystal of the square block pattern of even dispersion, a length of 2~3 μm of the crystal, width is 2~3 μm, a height of 0.2~1 μm.
Technical solution provided by the invention, with following the utility model has the advantages that (1) present invention utilizes ethylenediamine tetra-acetic acid for the first time
Disodium is adsorbed on cerous carbonate plane of crystal using the complexing power of itself and cerium ion as template, by Lattice Matching and stands
Body chemical structure complementation has the function of that space orientation and space constraint (utilize COO-With Ce3+Complexing forms cerous carbonate
Forming core site controls cerous carbonate crystallization unit self assembling process, NH by the way that the precipitating reagent containing carbonate is added2Base is adsorbed on carbonic acid
Cerium crystal surface), nucleation process and crystal growth etc. are controlled, so that the size of carbonic acid cerium crystal, pattern, structure are all controlled
And adjusting；(2) the liquid-phase precipitation system of present invention simulation biomineralization environment prepares blocky carbonic acid cerium crystal, entire reaction process
It carries out at room temperature, reaction condition is mild, and method is simple, easily controllable.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Fig. 1 is the SEM figure for the blocky carbonic acid cerium crystal being prepared in the embodiment of the present invention one；
Fig. 2 is the SEM figure for the blocky carbonic acid cerium crystal being prepared in the embodiment of the present invention two；
Fig. 3 is the SEM figure for the blocky carbonic acid cerium crystal being prepared in the embodiment of the present invention three；
Fig. 4 is the SEM figure for the blocky carbonic acid cerium crystal being prepared in the embodiment of the present invention four；
Fig. 5 is the SEM figure for the random flake cerium carbonate crystal being prepared in comparative example of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description.The following examples are only intended to illustrate the technical solution of the present invention more clearly, therefore is intended only as example, without
It can be limited the scope of the invention with this.
Experimental method in following embodiments is unless otherwise specified conventional method.Examination as used in the following examples
Material is tested, is to be commercially available from conventional reagent shop unless otherwise specified.Quantitative test in following embodiment, is all provided with
Three repeated experiments are set, data are the average value or mean+SD of three repeated experiments.(the NH that the present invention uses4)2CO3、NH4HCO3Purchased from three factory of Tianjin reagent, disodium ethylene diamine tetraacetate has purchased from Tianjin hearsay chemical reagent science and technology
Limit company, ethyl alcohol are analysis net product.
Blocky carbonic acid cerium crystal provided by the invention and preparation method thereof is made furtherly combined with specific embodiments below
It is bright.
Embodiment one
The present embodiment provides a kind of preparation methods of blocky carbonic acid cerium crystal, include the following steps:
S1: compound concentration is the cerous nitrate solution of 1.90mol/L, takes solution 15mL in 3000ml beaker, adds water to
580ml；Template disodium ethylene diamine tetraacetate 2.16g is weighed, cerium solution is added and is stirred until homogeneous, adjusting pH value is 3.5, is obtained
Mixed liquor, and in mixed liquor, Ce3+Molar concentration be 0.05mol/L, the concentration of disodium ethylene diamine tetraacetate is 3.72g/L；
S2: weighing precipitating reagent ammonium carbonate 7.5g, adds water 580mL to dissolve, is uniformly mixed, is entered with peristaltic pump in mixed liquor
The aqueous solution of precipitating reagent ammonium carbonate, feed time 3h continue to stir 0.5h after the completion of charging, are aged 4h；
S3: the product that ageing is obtained filters, and collects filter cake；Filter cake is washed 3 times using deionized water, then alcohol washes 2
It is secondary；Filter cake after alcohol is washed obtains blocky carbonic acid cerium crystal in 60 DEG C of drying 2h.
As a result: obtained carbonic acid cerium crystal is blocky carbonic acid cerium crystal, specific as shown in Figure 1.
Embodiment two
The present embodiment provides a kind of preparation methods of blocky carbonic acid cerium crystal, include the following steps:
S1: compound concentration is the cerous acetate solution of 0.90mol/L, takes solution 32mL in 3000ml beaker, adds water to
580mL；Template disodium ethylene diamine tetraacetate 2.16g is weighed, cerium solution is added and is stirred until homogeneous, adjusting pH value is 4, is mixed
Liquid is closed, and in mixed liquor, Ce3+Molar concentration be 0.05mol/L, the concentration of disodium ethylene diamine tetraacetate is 3.72g/L；
S2: weighing precipitating reagent ammonium carbonate 7.5g, adds water 1900mL to dissolve, is uniformly mixed, with peristaltic pump in mixed liquor
Enter the aqueous solution of precipitating reagent ammonium carbonate, feed time 3h continues to stir 0.5h after the completion of charging, is aged 4h；
S3: the product that ageing is obtained filters, and collects filter cake；Filter cake is washed 3 times using deionized water, then alcohol washes 2
It is secondary；Filter cake after alcohol is washed obtains blocky carbonic acid cerium crystal in 60 DEG C of drying 2h.
As a result: obtained carbonic acid cerium crystal is blocky carbonic acid cerium crystal, specific as shown in Figure 2.
Embodiment three
The present embodiment provides a kind of preparation methods of blocky carbonic acid cerium crystal, include the following steps:
S1: compound concentration is the cerous nitrate solution of 1.90mol/L, takes solution 16mL in 3000ml beaker, adds water to
580ml；Template disodium ethylene diamine tetraacetate 4.32g is weighed, cerium solution is added and is stirred until homogeneous, adjusting pH value is 3.5, is obtained
Mixed liquor, and in mixed liquor, Ce3+Molar concentration be 0.05mol/L, the concentration of disodium ethylene diamine tetraacetate is 7.45g/L；
S2: weighing precipitating reagent ammonium carbonate 7.5g, adds water 1900mL to dissolve, is uniformly mixed, with peristaltic pump in mixed liquor
Enter the aqueous solution of precipitating reagent ammonium carbonate, feed time 3h continues to stir 0.5h after the completion of charging, is aged 4h；
S3: the product that ageing is obtained filters, and collects filter cake；Filter cake is washed 3 times using deionized water, then alcohol washes 2
It is secondary；Filter cake after alcohol is washed obtains blocky carbonic acid cerium crystal in 60 DEG C of drying 2h.
As a result: obtained carbonic acid cerium crystal is blocky carbonic acid cerium crystal, specific as shown in Figure 3.
Example IV
The present embodiment provides a kind of preparation methods of blocky carbonic acid cerium crystal, include the following steps:
S1: compound concentration is the cerous nitrate solution of 1.90mol/L, takes solution 16mL in 3000ml beaker, adds water to
580ml；Template disodium ethylene diamine tetraacetate 6.49g is weighed, cerium solution is added and is stirred until homogeneous, adjusting pH value is 3.5, is obtained
Mixed liquor, and in mixed liquor, Ce3+Molar concentration be 0.05mol/L, the concentration of disodium ethylene diamine tetraacetate is 11.2g/L；
S2: weighing precipitating reagent ammonium carbonate 7.5g, adds water 1900mL to dissolve, is uniformly mixed, with peristaltic pump in mixed liquor
Enter the aqueous solution of precipitating reagent ammonium carbonate, feed time 3h continues to stir 0.5h after the completion of charging, is aged 4h；
S3: the product that ageing is obtained filters, and collects filter cake；Filter cake is washed 3 times using deionized water, then alcohol washes 2
It is secondary；Filter cake after alcohol is washed obtains blocky carbonic acid cerium crystal in 60 DEG C of drying 2h.
As a result: obtained carbonic acid cerium crystal is blocky carbonic acid cerium crystal, specific as shown in Figure 4.
Comparative example
This comparative example provides a kind of preparation method of carbonic acid cerium crystal, includes the following steps:
S1: compound concentration is the cerous nitrate solution of 1.90mol/L, takes solution 16mL in 3000ml beaker, adds water to
580ml makes Ce3+Molar concentration be 0.05mol/L；
S2: weighing precipitating reagent ammonium carbonate 7.5g, adds water 1900mL to dissolve, is uniformly mixed, with peristaltic pump in mixed liquor
Enter the aqueous solution of precipitating reagent ammonium carbonate, feed time 3h continues to stir 0.5h after the completion of charging, is aged 4h；
S3: the product that ageing is obtained filters, and collects filter cake；Filter cake is washed 3 times using deionized water, then alcohol washes 2
It is secondary；Filter cake after alcohol is washed obtains random flake cerium carbonate crystal in 60 DEG C of drying 2h.
As a result: obtained carbonic acid cerium crystal is random flake cerium carbonate crystal, specific as shown in Figure 5.
It should be noted that the case where enumerating in addition to above-described embodiment one to example IV, selects other preparation methods
Parameter is also feasible.
Technical solution provided by the invention, with following the utility model has the advantages that (1) present invention utilizes ethylenediamine tetra-acetic acid for the first time
Disodium is adsorbed on cerous carbonate plane of crystal using the complexing power of itself and cerium ion as template, by Lattice Matching and stands
Body chemical structure complementation has the function of that space orientation and space constraint (utilize COO-With Ce3+Complexing forms cerous carbonate
Forming core site controls cerous carbonate crystallization unit self assembling process, NH by the way that the precipitating reagent containing carbonate is added2Base is adsorbed on carbonic acid
Cerium crystal surface), nucleation process and crystal growth etc. are controlled, so that the size of carbonic acid cerium crystal, pattern, structure are all controlled
And adjusting；(2) the liquid-phase precipitation system of present invention simulation biomineralization environment prepares blocky carbonic acid cerium crystal, entire reaction process
It carries out at room temperature, reaction condition is mild, and method is simple, easily controllable.
It should be noted that unless otherwise indicated, technical term or scientific term used in this application should be this hair
The ordinary meaning that bright one of ordinary skill in the art are understood.Unless specifically stated otherwise, it otherwise illustrates in these embodiments
Component and opposite step, numerical expression and the numerical value of step are not limit the scope of the invention.It is illustrated and described herein
In all examples, unless otherwise prescribed, any occurrence should be construed as merely illustratively, not as limitation, because
This, other examples of exemplary embodiment can have different values.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme should all cover in protection scope of the present invention.
Claims (5)
1. a kind of preparation method of bulk carbonic acid cerium crystal, which comprises the steps of:
S1: being added template in cerium solution, is uniformly mixed, and adjusts pH value to 3~5, obtains mixed liquor；Wherein, the mould
Plate agent is disodium ethylene diamine tetraacetate, and the concentration of the template is 3~12g/L；Wherein, the cerium salt is water-soluble cerium
Salt, water-soluble cerium salt include one of cerous nitrate, cerium chloride, cerous acetate and cerous sulfate or a variety of；
S2: the aqueous solution of precipitating reagent is added in the mixed liquor, is aged after stirring；Wherein, the precipitating reagent and described
The mass ratio of cerium salt is 1:(0.5~2), the molar concentration of precipitating reagent is 0.04~0.58mol/ in the aqueous solution of the precipitating reagent
L；The precipitating reagent is soluble carbonate salt, and the soluble carbonate salt includes ammonium carbonate, ammonium hydrogen carbonate, sodium carbonate and bicarbonate
One of sodium is a variety of；
S3: the obtained product that is aged successively is filtered, washed and dried, evenly dispersed square block pattern is obtained
Carbonic acid cerium crystal, a length of 2~3 μm of the crystal of the carbonic acid cerium crystal, width is 2~3 μm, a height of 0.2~1 μm.
2. the preparation method of bulk carbonic acid cerium crystal according to claim 1, it is characterised in that:
In the mixed liquor of the S1, Ce3+Molar concentration be 0.05~0.58mol/L.
3. the preparation method of bulk carbonic acid cerium crystal according to claim 1, it is characterised in that:
Described to be incorporated as being slowly added in the S2, the time of adition process is 0.5~4h；The time of the stirring is 0.5h.
4. the preparation method of bulk carbonic acid cerium crystal according to claim 1, it is characterised in that:
In the S2, the time of the ageing is 0.5~48h.
5. the preparation method of bulk carbonic acid cerium crystal according to claim 1, it is characterised in that:
The S3 is specifically included: the obtained product that is aged being filtered, filter cake is collected；The filter cake is clear using deionized water
It washes 3 times, then alcohol is washed 2 times；Filter cake after the alcohol is washed obtains the blocky carbonic acid cerium crystal in 60 DEG C of drying 2h.
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| CN112126977B (en) * | 2020-08-11 | 2021-11-19 | 南昌大学 | Method for preparing high-purity flaky single crystal and flaky crystal dense aggregated cerium carbonate |
| CN114082396B (en) * | 2021-09-28 | 2023-07-11 | 淮阴师范学院 | Magnetic persimmon cake-shaped cerium ferrite/cerium dioxide composite adsorbent and preparation method thereof |
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| CN103214015B (en) * | 2013-04-12 | 2014-11-26 | 内蒙古科技大学 | Method for regulating and controlling synthesized petaloid cerium oxide by utilizing cationic polyelectrolyte template |
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