CN107098374A - Dispersed bulk morphologies carbonic acid cerium crystal and preparation method thereof - Google Patents
Dispersed bulk morphologies carbonic acid cerium crystal and preparation method thereof Download PDFInfo
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- CN107098374A CN107098374A CN201710381052.1A CN201710381052A CN107098374A CN 107098374 A CN107098374 A CN 107098374A CN 201710381052 A CN201710381052 A CN 201710381052A CN 107098374 A CN107098374 A CN 107098374A
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- carbonic acid
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
Abstract
The present invention relates to a kind of preparation method of block carbonic acid cerium crystal, it is in simulation biomineralization environmental system, it is raw material for soft template, soluble cerium salt to use disodium ethylene diamine tetraacetate, soluble carbonate salt is precipitating reagent, by mixing, ageing, filtering, washing and baking step, the carbonic acid cerium crystal of dispersed bulk morphologies is prepared.The present invention is using the space complexing power of disodium ethylene diamine tetraacetate, and complementary by Lattice Matching and spatial chemistry, nucleation and crystal growth to cerous carbonate regulate and control, and have obtained the carbonic acid cerium crystal of granularity, pattern and structure-controllable；Preparation method has that low in raw material price, reaction condition be gentle, the low feature of energy consumption, is adapted to industrialized production.
Description
Technical field
The present invention relates to powder body material technical field, and in particular to a kind of dispersed bulk morphologies carbonic acid cerium crystal and
Its preparation method.
Background technology
Baotou rare earth aboundresources, and the characteristics of Baotou rare earth resource occupied an leading position with light rare earth, wherein cerium contains
Amount accounts for 50%, therefore exploitation cerium resources advantage is particularly important.Cerium oxide has the property of N-type semiconductor, the 4f electronics for having uniqueness
Structure, show it is excellent store oxygen ability and charge-exchange ability, be widely used in three-way catalyst, fuel cell, light and urge
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 are special physical property, pattern, size, structure, dispersiveness, the surface property of such as particle, these physical and chemical performances determine that it is applied
Field, therefore, seeks eased controllable preparation method just very necessary.Mineralization method introducing is prepared into special appearance
Cerium oxide, be expected to realize effective control of the pattern of cerium oxide, size distribution and structure.Ceria during due to low-temperature bake
Pattern there is heredity, so can just control the pattern of cerium oxide by the cerous carbonate for synthesizing special appearance.Template is made
For synthetic material controlling agent, the self assembling process of material directly take part in.At present, ball has been prepared using different templates
The cerium oxide of shape, bar-shaped and flower-shaped etc. different-shape, as block carbonic acid cerium crystal, has not been reported.
The content of the invention
For defect of the prior art, present invention aims at providing, a kind of dispersed bulk morphologies cerous carbonate is brilliant
Body and preparation method thereof, with by using the complexing and space structure of disodium ethylene diamine tetraacetate, by Lattice Matching and
Stereochemical structure complementation control cerous carbonate nucleation process and crystal growth, obtain particle size uniformity, the bulk of pattern rule
Shape carbonic acid cerium crystal；Whole course of reaction is carried out at room temperature, and reaction condition is gentle, and method is simple, it is easy to control.
To achieve the above object, the technical scheme that provides of the present invention is：
In a first aspect, the invention provides a kind of preparation method of block carbonic acid cerium crystal, comprising the following steps：S1：
Template is added in cerium solution, is well mixed, regulation pH value obtains mixed liquor to 3~5；S2：Precipitation is added in mixed liquor
It is aged after the aqueous solution of agent, stirring；S3：The product that ageing is obtained is filtered, washed and dried successively, obtains bulk
Carbonic acid cerium crystal.It should be noted that in S1 and S2, the process of addition can be with constantly stirring.
In the further embodiment of the present invention, in S1 mixed liquor, Ce3+Molar concentration be 0.05~0.58mol/
L, the concentration of template is 3~12g/L.
In the further embodiment of the present invention, in S2, the mass ratio of precipitating reagent and cerium salt is 1:(0.5~2), precipitation
The molar concentration of precipitating reagent is 0.04~0.58mol/L in the aqueous solution of agent.
In the further embodiment of the present invention, in S2, be incorporated as being slowly added to, time of adition process for 0.5~
4h；The time of stirring is 0.5h.
In the further embodiment of the present invention, in S2, the time of ageing is 0.5~48h.
In the further embodiment of the present invention, in S1, cerium salt is water-soluble cerium salt, water-soluble cerium salt bag
Include the one or more in cerous nitrate, cerium chloride, cerous acetate and cerous sulfate.
In the further embodiment of the present invention, in S2, precipitating reagent is soluble carbonate salt, and soluble carbonate salt includes
One or more in ammonium carbonate, ammonium hydrogen carbonate, sodium carbonate and sodium acid carbonate.
In the further embodiment of the present invention, in S1, template is disodium ethylene diamine tetraacetate.
In the further embodiment of the present invention, S3 is specifically included：Obtained product filtering will be aged, collects filter cake；
Filter cake is used into deionized water washing 3 times, then alcohol is washed 2 times；Filter cake after alcohol is washed dries 2h at 60 DEG C, obtains block carbonic acid
Cerium crystal.
Second aspect, the invention provides the block cerous carbonate that the preparation method using block 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 is raw material, adds the precipitating reagent containing carbonate, by ageing, filtering, drying, has been prepared
The carbonic acid cerium crystal of even scattered square block pattern, a length of 2~3 μm, a width of 2~3 μm, a height of 0.2~1 μm of the crystal.
The technical scheme that the present invention is provided, with following beneficial effect：(1) present invention utilizes ethylenediamine tetra-acetic acid first
Disodium is as template, using its complexing power with cerium ion, and absorption is in cerous carbonate plane of crystal, by Lattice Matching and vertical
There is the complementation of body chemical constitution space orientation and the effect of space constraint (to utilize COO-With Ce3+Complexing formation cerous carbonate
Forming core site, cerous carbonate crystallization unit self assembling process, NH are controlled by adding the precipitating reagent containing carbonate2Base is adsorbed in carbonic acid
Cerium crystal surface), control nucleation process and crystal growth etc. so that size, pattern, the structure of carbonic acid cerium crystal are all controlled
And regulation；(2) the liquid-phase precipitation system of present invention simulation biomineralization environment prepares block carbonic acid cerium crystal, whole course of reaction
Carry out at room temperature, reaction condition is gentle, and method is simple, it is easy to control.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Brief description of the drawings
Fig. 1 is the SEM figures of the block carbonic acid cerium crystal prepared in the embodiment of the present invention one；
Fig. 2 is the SEM figures of the block carbonic acid cerium crystal prepared in the embodiment of the present invention two；
Fig. 3 is the SEM figures of the block carbonic acid cerium crystal prepared in the embodiment of the present invention three；
Fig. 4 is the SEM figures of the block carbonic acid cerium crystal prepared in the embodiment of the present invention four；
Fig. 5 is the SEM figures of the random flake cerium carbonate crystal prepared in comparative example of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described.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 conventional method unless otherwise specified.Examination used in following embodiments
Material is tested, is to be commercially available from conventional reagent shop unless otherwise specified.Quantitative test in following examples, is all provided with
Three repetition experiments are put, data are the average value or mean+SD of three repetition experiments.(the NH that the present invention is used4)2CO3、NH4HCO3Purchased from the factory of Tianjin reagent three, disodium ethylene diamine tetraacetate has purchased from Tianjin hearsay chemical reagent science and technology
Limit company, ethanol is analysis net product.
Block carbonic acid cerium crystal provided with reference to specific embodiment the present invention and preparation method thereof is made furtherly
It is bright.
Embodiment one
The present embodiment provides a kind of preparation method of block carbonic acid cerium crystal, comprises the following steps：
S1：Compound concentration is 1.90mol/L cerous nitrate solution, takes solution 15mL in 3000ml beakers, adds water to
580ml；Template disodium ethylene diamine tetraacetate 2.16g is weighed, cerium solution is added and is stirred until homogeneous, it is 3.5 to adjust pH value, is obtained
In mixed liquor, and mixed liquor, Ce3+Molar concentration be 0.05mol/L, the concentration of disodium ethylene diamine tetraacetate is 3.72g/L；
S2：Precipitating reagent ammonium carbonate 7.5g, the 580mL that adds water dissolving is weighed, is uniformly mixed, is entered with peristaltic pump in mixed liquor
The aqueous solution of precipitating reagent ammonium carbonate, feed time is 3h, continues to stir 0.5h after the completion of charging, is aged 4h；
S3：Obtained product filtering will be aged, 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 dries 2h at 60 DEG C, obtains block carbonic acid cerium crystal.
As a result：Obtained carbonic acid cerium crystal is block carbonic acid cerium crystal, specific as shown in Figure 1.
Embodiment two
The present embodiment provides a kind of preparation method of block carbonic acid cerium crystal, comprises the following steps：
S1：Compound concentration is 0.90mol/L cerous acetate solution, takes solution 32mL in 3000ml beakers, adds water to
580mL；Template disodium ethylene diamine tetraacetate 2.16g is weighed, cerium solution is added and is stirred until homogeneous, it is 4 to adjust pH value, is mixed
Close in liquid, and mixed liquor, Ce3+Molar concentration be 0.05mol/L, the concentration of disodium ethylene diamine tetraacetate is 3.72g/L；
S2：Precipitating reagent ammonium carbonate 7.5g, the 1900mL that adds water dissolving is weighed, is uniformly mixed, with peristaltic pump in mixed liquor
Enter the aqueous solution of precipitating reagent ammonium carbonate, feed time is 3h, continue to stir 0.5h after the completion of charging, be aged 4h；
S3：Obtained product filtering will be aged, 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 dries 2h at 60 DEG C, obtains block carbonic acid cerium crystal.
As a result：Obtained carbonic acid cerium crystal is block carbonic acid cerium crystal, specific as shown in Figure 2.
Embodiment three
The present embodiment provides a kind of preparation method of block carbonic acid cerium crystal, comprises the following steps：
S1：Compound concentration is 1.90mol/L cerous nitrate solution, takes solution 16mL in 3000ml beakers, adds water to
580ml；Template disodium ethylene diamine tetraacetate 4.32g is weighed, cerium solution is added and is stirred until homogeneous, it is 3.5 to adjust pH value, is obtained
In mixed liquor, and mixed liquor, Ce3+Molar concentration be 0.05mol/L, the concentration of disodium ethylene diamine tetraacetate is 7.45g/L；
S2：Precipitating reagent ammonium carbonate 7.5g, the 1900mL that adds water dissolving is weighed, is uniformly mixed, with peristaltic pump in mixed liquor
Enter the aqueous solution of precipitating reagent ammonium carbonate, feed time is 3h, continue to stir 0.5h after the completion of charging, be aged 4h；
S3：Obtained product filtering will be aged, 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 dries 2h at 60 DEG C, obtains block carbonic acid cerium crystal.
As a result：Obtained carbonic acid cerium crystal is block carbonic acid cerium crystal, specific as shown in Figure 3.
Example IV
The present embodiment provides a kind of preparation method of block carbonic acid cerium crystal, comprises the following steps：
S1：Compound concentration is 1.90mol/L cerous nitrate solution, takes solution 16mL in 3000ml beakers, adds water to
580ml；Template disodium ethylene diamine tetraacetate 6.49g is weighed, cerium solution is added and is stirred until homogeneous, it is 3.5 to adjust pH value, is obtained
In mixed liquor, and mixed liquor, Ce3+Molar concentration be 0.05mol/L, the concentration of disodium ethylene diamine tetraacetate is 11.2g/L；
S2：Precipitating reagent ammonium carbonate 7.5g, the 1900mL that adds water dissolving is weighed, is uniformly mixed, with peristaltic pump in mixed liquor
Enter the aqueous solution of precipitating reagent ammonium carbonate, feed time is 3h, continue to stir 0.5h after the completion of charging, be aged 4h；
S3：Obtained product filtering will be aged, 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 dries 2h at 60 DEG C, obtains block carbonic acid cerium crystal.
As a result：Obtained carbonic acid cerium crystal is block 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, comprises the following steps：
S1：Compound concentration is 1.90mol/L cerous nitrate solution, takes solution 16mL in 3000ml beakers, adds water to
580ml, makes Ce3+Molar concentration be 0.05mol/L；
S2：Precipitating reagent ammonium carbonate 7.5g, the 1900mL that adds water dissolving is weighed, is uniformly mixed, with peristaltic pump in mixed liquor
Enter the aqueous solution of precipitating reagent ammonium carbonate, feed time is 3h, continue to stir 0.5h after the completion of charging, be aged 4h；
S3：Obtained product filtering will be aged, 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 dries 2h at 60 DEG C, obtains random flake cerium carbonate crystal.
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 situation about enumerating except above-described embodiment one to example IV, from other preparation methods
Parameter is also feasible.
The technical scheme that the present invention is provided, with following beneficial effect：(1) present invention utilizes ethylenediamine tetra-acetic acid first
Disodium is as template, using its complexing power with cerium ion, and absorption is in cerous carbonate plane of crystal, by Lattice Matching and vertical
There is the complementation of body chemical constitution space orientation and the effect of space constraint (to utilize COO-With Ce3+Complexing formation cerous carbonate
Forming core site, cerous carbonate crystallization unit self assembling process, NH are controlled by adding the precipitating reagent containing carbonate2Base is adsorbed in carbonic acid
Cerium crystal surface), control nucleation process and crystal growth etc. so that size, pattern, the structure of carbonic acid cerium crystal are all controlled
And regulation；(2) the liquid-phase precipitation system of present invention simulation biomineralization environment prepares block carbonic acid cerium crystal, whole course of reaction
Carry out at room temperature, reaction condition is gentle, and method is simple, it is easy to control.
It should be noted that unless otherwise indicated, technical term or scientific terminology 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, otherwise illustrate in these embodiments
Part and relative 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 exemplary, not as limitation, because
This, other examples of exemplary embodiment can have different values.
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, or which part or all technical characteristic are entered
Row equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme, it all should cover among protection scope of the present invention.
Claims (10)
1. a kind of preparation method of block carbonic acid cerium crystal, it is characterised in that comprise the following steps：
S1：Template is added in cerium solution, is well mixed, regulation pH value obtains mixed liquor to 3~5；
S2：The aqueous solution of precipitating reagent is added in the mixed liquor, is aged after stirring；
S3：The product that the ageing is obtained is filtered, washed and dried successively, obtains the block carbonic acid cerium crystal.
2. the preparation method of block 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, the concentration of template is 3~12g/
L。
3. the preparation method of block carbonic acid cerium crystal according to claim 1, it is characterised in that：
In the S2, the mass ratio of the precipitating reagent and the cerium salt is 1:Sunk in (0.5~2), the aqueous solution of the precipitating reagent
The molar concentration of shallow lake agent is 0.04~0.58mol/L.
4. the preparation method of block 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.
5. the preparation method of block 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.
6. the preparation method of block carbonic acid cerium crystal according to claim 1, it is characterised in that：
In the S1, the cerium salt is water-soluble cerium salt, and water-soluble cerium salt includes cerous nitrate, cerium chloride, vinegar
One or more in sour cerium and cerous sulfate.
7. the preparation method of block carbonic acid cerium crystal according to claim 1, it is characterised in that：
In the S2, the precipitating reagent is soluble carbonate salt, and the soluble carbonate salt includes ammonium carbonate, ammonium hydrogen carbonate, carbon
One or more in sour sodium and sodium acid carbonate.
8. the preparation method of block carbonic acid cerium crystal according to claim 1, it is characterised in that：
In the S1, the template is disodium ethylene diamine tetraacetate.
9. the preparation method of block carbonic acid cerium crystal according to claim 1, it is characterised in that：
The S3 is specifically included：By the product filtering for being aged and obtaining, filter cake is collected；The filter cake is clear using deionized water
Wash 3 times, then alcohol is washed 2 times；Filter cake after the alcohol is washed dries 2h at 60 DEG C, obtains the block carbonic acid cerium crystal.
10. the block carbonic acid cerium crystal that the preparation method described in claim any one of 1-9 is prepared.
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Cited By (3)
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| CN107601545A (en) * | 2017-10-23 | 2018-01-19 | 常州市卓群纳米新材料有限公司 | A kind of preparation method of bulky grain cerous carbonate |
| CN112126977A (en) * | 2020-08-11 | 2020-12-25 | 南昌大学 | Method for preparing high-purity flaky single crystal and flaky crystal dense aggregated cerium carbonate |
| CN114082396A (en) * | 2021-09-28 | 2022-02-25 | 淮阴师范学院 | Magnetic persimmon cake-shaped cerium ferrite/cerium dioxide composite adsorbent and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601545A (en) * | 2017-10-23 | 2018-01-19 | 常州市卓群纳米新材料有限公司 | A kind of preparation method of bulky grain cerous carbonate |
| CN112126977A (en) * | 2020-08-11 | 2020-12-25 | 南昌大学 | Method for preparing high-purity flaky single crystal and flaky crystal dense aggregated cerium carbonate |
| CN114082396A (en) * | 2021-09-28 | 2022-02-25 | 淮阴师范学院 | Magnetic persimmon cake-shaped cerium ferrite/cerium dioxide composite adsorbent and preparation method thereof |
| 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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