CN103641147B - A kind of preparation method of micron-order ellipsoidal cerium oxide - Google Patents
A kind of preparation method of micron-order ellipsoidal cerium oxide Download PDFInfo
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- CN103641147B CN103641147B CN201310646000.4A CN201310646000A CN103641147B CN 103641147 B CN103641147 B CN 103641147B CN 201310646000 A CN201310646000 A CN 201310646000A CN 103641147 B CN103641147 B CN 103641147B
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- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 46
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 63
- 239000002245 particle Substances 0.000 claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 20
- 150000000703 Cerium Chemical class 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000000877 morphologic effect Effects 0.000 claims abstract description 5
- 238000013021 overheating Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical group [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 12
- 239000012452 mother liquor Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000001556 precipitation Methods 0.000 claims description 9
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 8
- 239000003755 preservative agent Substances 0.000 claims description 8
- 230000002335 preservative effect Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims description 2
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 2
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
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- 239000006096 absorbing agent Substances 0.000 abstract description 5
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- 239000007864 aqueous solution Substances 0.000 abstract description 3
- 239000000919 ceramic Substances 0.000 abstract description 2
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- 238000001338 self-assembly Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract 1
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- 239000000243 solution Substances 0.000 description 27
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- 150000002500 ions Chemical class 0.000 description 7
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- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002808 molecular sieve Substances 0.000 description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000013335 mesoporous material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- -1 polyoxyethylene Polymers 0.000 description 2
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 description 2
- 102100030310 5,6-dihydroxyindole-2-carboxylic acid oxidase Human genes 0.000 description 1
- 241000024287 Areas Species 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 101000773083 Homo sapiens 5,6-dihydroxyindole-2-carboxylic acid oxidase Proteins 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
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- 230000008844 regulatory mechanism Effects 0.000 description 1
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- 239000012266 salt solution Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of preparation method of micron-order ellipsoidal cerium oxide, it adopts gas-to-liquid contact method, and solubility cerium salt is as raw material, and CTAB is as Morphological control agent, and at room temperature, the micella that the CTAB in the aqueous solution is formed is by positively charged head base CTA
+with CO
3 2-electrostatic matching effect induce the self-assembly of presoma, change the habit of presoma, thus affect the pattern of presoma, finally control the physical property such as the pattern of product cerium oxide and size through Overheating Treatment.Finally prepare axiolitic granular precursor, obtain after roasting dispersed better, the micron order ellipsoid shape cerium oxide particle of uniform particle sizes, products obtained therefrom particle major axis is about 9 μm, and it is 6 μm that minor axis is about, and diameter of axle ratio is about 1.5.The cerium oxide particle of this method gained in water treatment catalytic purification, electronic ceramics, uv-absorbing agent etc. in have important effect.
Description
Technical field
The present invention relates to a kind of preparation method of elliposoidal cerium dioxide, specifically in gas-to-liquid contact method reaction unit, utilize cetyl trimethylammonium bromide (CTAB) to regulate and control to prepare the method for powder as morphology control agent, belong to field of micro-nano material technology.
Background technology
Cerium oxide is as a kind of light rare earths oxide compound of having many uses, and it has the chemical property of N-type semiconductor.The special physicochemical property of cerium dioxide directly may affect the performance of material, as added cerium dioxide in pottery, not only obviously can reduce the sintering temperature of pottery, and can improve the density of pottery.Because Ce element has appraising at the current rate property, cerium oxide also plays important effect in field of light emitting materials.The absorption bands major part of cerium oxide is in ultraviolet region, is widely used in the fields such as uv-absorbing agent, luminescent material, glass polishing agent, auto-exhaust catalyst, electronic ceramics.
Along with the progress of science and technology, the requirement for cerium oxide powder material is more and more higher.In many Application Areass, two important requirements are exactly size, the pattern of cerium oxide powder.Therefore, the cerium oxide powder material that preparation size is even, pattern is reproducible, degree of crystallinity is high, has widened the application of cerium oxide in uv-absorbing agent, fluorescence luminescent material etc.
The report that current use cetyl trimethylammonium bromide (CTAB) does template is a lot, generally all utilizes hydrothermal method to come synthesising mesoporous molecular sieve, mesoporous material etc.Li Fuxiang etc. take CTAB as template, zirconium nitrate is raw material, have successfully prepared Mesoporous Zirconia Molecular Sieve (petrochemical complex, 2005,34 (12), 1129-1133) in dehydrated alcohol; Zhao Yongjie etc. are mixed into template with CATB and polyoxyethylene glycol, obtain thick hole wall ordered mesoporous material (daily chemical industry, 2010,40 (6), 435-438) through de-to wash, after the art breading such as roasting; Wang Shanshan etc. take CTAB as template, adopt hydrothermal method to synthesize the molecular sieve (modern chemical industry, 2011,31 (2), 75-79) that stability is better, order is stronger in the short period of time.
Gas-to-liquid contact method refers to and utilizes volatile salt, bicarbonate of ammonia etc. slowly to decompose the CO produced
2gas slowly diffuses in soluble metal salt solution, dissolves and forms CO
3 2-and belong to salt ion generation precipitin reaction with GOLD FROM PLATING SOLUTION and generate presoma, then prepare powder body material through super-dry, roasting.
At present, cetyl trimethylammonium bromide (CTAB) regulates and controls synthesis special appearance and the CeO of size for template
2material all have employed the prevailing method liquid phase method of nano materials substantially.
Summary of the invention
The technical issues that need to address of the present invention are just the defect overcoming prior art, a kind of preparation method of micron-order ellipsoidal cerium oxide is provided, it selects cetyl trimethylammonium bromide (CTAB) as Morphological control agent, adopt gas-to-liquid contact method, prepare the granular precursor of elliposoidal, then obtain after high-temperature heat treatment dispersed better, the micron order ellipsoid shape cerium oxide particle of uniform particle sizes, products obtained therefrom particle major axis is about 9 μm, it is 6 μm that minor axis is about, and diameter of axle ratio is about 1.5.The size uniform prepared, the ellipsoidal cerium oxide powder body material that pattern is reproducible, degree of crystallinity is high have widened the application of cerium oxide in uv-absorbing agent, fluorescence luminescent material etc.
For solving the problem, the present invention adopts following technical scheme:
The invention provides a kind of preparation method of micron-order ellipsoidal cerium oxide, described method is for selecting cetyl trimethylammonium bromide (CTAB) as Morphological control agent, adopt gas-to-liquid contact method, prepare the granular precursor of elliposoidal, obtain after Overheating Treatment more dispersed better, the micron order ellipsoid shape cerium oxide particle of uniform particle sizes, products obtained therefrom particle major axis is 7-11 μm, and minor axis is about as 4-8 μm, and diameter of axle ratio is about 1.2-1.6.
Concrete steps are as follows:
(1) compound concentration is the cerium salt mother liquor of 220.97g/L, and get this mother liquor 7.8ml-62.2ml in beaker, add water to 500ml, adjust pH is 4; Take cetyl trimethylammonium bromide (CTAB) pressed powder, add water 500ml, and under 40 DEG C of conditions, heating makes it fully dissolve in 1 minute, stirs and makes it be uniformly dispersed;
While stirring cerium salt mother liquor, cetyl trimethylammonium bromide (CTAB) solution is joined in cerium salt mother liquor, continue stirring 20 minutes, make the surfactant-dispersed in mixing solutions even, obtain the mixing solutions 1L that cerium solution that concentration is 0.01mol/l ~ 0.08 mol/L and concentration are the CTAB solution of 0.1 g/L ~ 3.0 g/L, the pH value regulating initial mixing solution is 3 ~ 5, is then sealed by beaker mouth with preservative film, pricks several hole;
(2) take 1.2 ~ 3 times that precipitation agent molar weight is corresponding cerium salt molar weight, after weighing up, make it be uniformly dispersed with mortar grinding powder, load in culture dish, with preservative film, culture dish collar extension is sealed simultaneously, prick several hole;
(3) beaker of the cerium salt in moisture eliminator and cetyl trimethylammonium bromide (CTAB) mixing solutions is put into the two-layer up and down of moisture eliminator respectively with the culture dish of dress precipitation agent, react 15 ~ 25 days in moisture eliminator, obtain elliposoidal granular precursor;
(4) elliposoidal granular precursor is through 400 ~ 1000 DEG C of roastings, obtains the cerium oxide particle of micron-order ellipsoidal.
In the present invention, cerium salt used is water-soluble cerium salt, and described water-soluble cerium salt is cerous nitrate, cerous sulfate, cerous acetate or Cerium II Chloride.
In the present invention, described precipitation agent is labile carbonate under the room temperature condition containing carbonate, and described is volatile salt or bicarbonate of ammonia containing labile carbonate under the room temperature condition of carbonate.
In the present invention, described tensio-active agent is that have in the aqueous solution can negatively charged ion CO brilliant in structure
3 2-, OH
-what electrostatic mated contains CTA
+the ammonium salt of ion, having in the described aqueous solution can negatively charged ion CO brilliant in structure
3 2-, OH
-what electrostatic mated contains CTA
+the ammonium salt of ion is cetyl trimethylammonium bromide (CTAB).
In the present invention, react after 15 ~ 25 days in moisture eliminator, replace washing sample three times by dehydrated alcohol and secondary deionized water, at 30-60 DEG C, drying obtains elliposoidal granular precursor.
In the present invention, elliposoidal granular precursor is 400 ~ 1000 DEG C of roastings, and heat-up rate 200 DEG C/h, soaking time 2h, cools to room temperature with the furnace, obtains micron-order ellipsoidal cerium oxide particle.
The present invention selects cetyl trimethylammonium bromide (CTAB) as Morphological control agent, adopt gas-to-liquid contact method, prepare the granular precursor of elliposoidal, obtain after high-temperature heat treatment more dispersed better, the micron order ellipsoid shape cerium oxide particle of uniform particle sizes, products obtained therefrom particle major axis is about 9 μm, it is 6 μm that minor axis is about, and diameter of axle ratio is about 1.5.
Advantage of the present invention:
The present invention adopts that reaction conditions is simply controlled, speed of response slowly, the gas-to-liquid contact method of the state geo-stationary of repeated high, the solution-air two-phase of stable, morphology microstructure regulates and controls to prepare cerium oxide precursor body and cerium oxide powder material in conjunction with cetyl trimethylammonium bromide (CTAB) template.In simultaneous test, gas-to-liquid contact method is not subject to the interference of other factors simultaneously, can fully play the control of cetyl trimethylammonium bromide (CTAB) for crystal morphology, better research CTAB is for the Regulation Mechanism of presoma crystal morphology and crystal formation.Cetyl trimethylammonium bromide (CTAB) in aqueous can ionize out can negatively charged ion (CO brilliant in structure
3 2-, OH
-) electrostatic coupling CTA
+ion, these CTA
+the surface being arranged in CTAB micella that ion meeting is directed, induction of the self-assembly of the granular precursor on surfactant micelle surface, changes the habit of presoma crystal, finally effectively plays the effect that template CTAB regulates and controls the pattern of granular precursor.The size uniform prepared, the ellipsoidal cerium oxide powder body material that pattern is reproducible, degree of crystallinity is high have widened the application of cerium oxide in uv-absorbing agent, fluorescence luminescent material etc.
Accompanying drawing explanation
Fig. 1 is gas-to-liquid contact subtraction unit schematic diagram.
Fig. 2 [Ce
3+] be 0.02mol/L, [CTAB] is 0.5g/L, and initial soln PH is 3, reacts 15 days, the SEM picture of the presoma of preparation.
Fig. 3 [Ce
3+] be 0.02mol/L, [CTAB] is 0.5g/L, and initial soln PH is 3, reacts 15 days, the SEM picture of the cerium oxide of 500 DEG C of roasting synthesis.
Fig. 4 [Ce
3+] be 0.03mol/L, [CTAB] is 1.5g/L, and initial soln PH is 5, reacts the infared spectrum (FT-IR) of the presoma of preparation in 15 days.
Fig. 5 [Ce
3+] be 0.03mol/L, [CTAB] is 1.5g/L, and initial soln PH is 5, reacts the X ray diffracting spectrum (XRD) of the presoma of preparation in 15 days.
Fig. 6 [Ce
3+] be 0.03mol/L, [CTAB] is 1.5g/L, and initial soln PH is 5, reacts 15 days, the SEM picture of the cerium oxide of 500 DEG C of roasting synthesis.
Fig. 7 [Ce
3+] be 0.03mol/L, [CTAB] is 1.5g/L, and initial soln PH is 5, reacts 15 days, the X ray diffracting spectrum (XRD) of the cerium oxide of 500 DEG C of roasting synthesis.
Embodiment
(NH used in the specific embodiment of the invention
4)
2cO
3, NH
4hCO
3for Tianjin reagent three factory analytical pure product, cetyl trimethylammonium bromide (CTAB) is Beijing chemical reagents corporation, and ethanol is analytical pure product.The reaction unit schematic diagram of gas-to-liquid contact method as shown in Figure 1.In Fig. 1,1 is moisture eliminator, and 2 for being equipped with the beaker of cerium solution, and 3 is precipitation agent, and 4 for adding the ammonia of beaker, and 5 for adding the carbonic acid gas of beaker.
embodiment 1
(1) compound concentration is the cerous nitrate mother liquor of 220.97g/L, and get this mother liquor 15.6ml in 1L beaker, add water to 500ml, adjust pH is 4; Take 0.5g cetyl trimethylammonium bromide (CTAB) pressed powder, add water 500ml, and under 40 DEG C of conditions, heating makes it fully dissolve in 1 minute, stirs and makes it be uniformly dispersed; While stirring cerous nitrate solution, gradually cetyl trimethylammonium bromide (CTAB) solution is joined in cerous nitrate solution and goes, continue stirring 20 minutes, make the surfactant-dispersed in mixing solutions even, obtain the mixing solutions 1L that cerous nitrate solution that concentration is 0.02mol/l and concentration are the CTAB solution of 0.5 g/l, the pH value adjusting initial mixing solution is 3, is then sealed by beaker mouth with preservative film, pricks 3 holes;
(2) take precipitation agent bicarbonate of ammonia 4.74 g, use mortar grinding powder, load in culture dish, seal culture dish collar extension simultaneously with preservative film, 3 holes are pricked on surface;
(3) culture dish of the beaker filling cerous nitrate and CTAB mixing solutions in moisture eliminator and dress volatile salt is placed in the two-layer up and down of moisture eliminator respectively, confined reaction, after 15 days, obtains elliposoidal granular precursor;
(4) elliposoidal granular precursor is through retort furnace roasting, within 2.5 hours, is warmed up to 500 DEG C, and be incubated 2 hours, furnace cooling is to room temperature afterwards, obtains spheroid shape cerium oxide particle, obtains the cerium oxide particle of elliposoidal; Carry out SEM test to the presoma that this example synthesizes, as shown in Figure 2, the cerium oxide SEM picture that roasting obtains, as shown in Figure 3, ellipsoid shape cerium oxide particle is dispersed better, uniform particle sizes, particle size are micron order.
embodiment 2
(1) compound concentration is the cerous nitrate mother liquor of 220.97g/L, and get this mother liquor 23.4ml in 1L beaker, add water to 500ml, adjust pH is 4; Take 1.5g cetyl trimethylammonium bromide (CTAB) pressed powder, add water 500ml, and under 40 DEG C of conditions, heating makes it fully dissolve in 1 minute, stirs and makes it be uniformly dispersed; While stirring cerous nitrate solution, gradually cetyl trimethylammonium bromide (CTAB) solution is joined in cerous nitrate solution and goes, continue stirring 20 minutes, make the surfactant-dispersed in mixing solutions even, obtain the mixing solutions 1L that cerous nitrate solution that concentration is 0.03mol/l and concentration are the CTAB solution of 1.5 g/l, the pH value adjusting initial mixing solution is 5, is then sealed by beaker mouth with preservative film, pricks 3 holes;
(2) take precipitation agent volatile salt 8.64g, use mortar grinding powder, load in culture dish, seal culture dish collar extension simultaneously with preservative film, 3 holes are pricked on surface;
(3) culture dish of the beaker filling cerous nitrate and CTAB mixing solutions in moisture eliminator and dress volatile salt is placed in the two-layer up and down of moisture eliminator respectively, confined reaction, after 15 days, obtains elliposoidal granular precursor;
(4) elliposoidal granular precursor is through retort furnace roasting, within 2.5 hours, is warmed up to 500 DEG C, and be incubated 2 hours, furnace cooling is to room temperature afterwards, obtains spheroid shape cerium oxide particle, obtains the cerium oxide particle of elliposoidal; The presoma that this example obtains carries out infrared, X-ray diffraction test, result, as shown in Figure 4 and Figure 5; The cerium oxide that this example roasting obtains carries out SEM, X-ray diffraction test, and as shown in Figure 6 and Figure 7, ellipsoid shape cerium oxide particle product major axis is about 9 μm, and it is 6 μm that minor axis is about, and diameter of axle ratio is about 1.5.
Last it is noted that obviously, above-described embodiment is only for example of the present invention is clearly described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of amplifying out or variation be still among protection scope of the present invention.
Claims (6)
1. the preparation method of a micron-order ellipsoidal cerium oxide, it is characterized in that, described method is for selecting cetyl trimethylammonium bromide (CTAB) as Morphological control agent, adopt gas-to-liquid contact method, prepare the granular precursor of elliposoidal, then obtain after Overheating Treatment dispersed better, the micron order ellipsoid shape cerium oxide particle of uniform particle sizes, products obtained therefrom particle major axis is 7-11 μm, minor axis is long is 4-8 μm, and the diameter of axle is than being 1.2-1.6.
2.
the preparation method of micron-order ellipsoidal cerium oxide as claimed in claim 1, is characterized in that, concrete steps are as follows:
(1) compound concentration is the cerium salt mother liquor of 220.97g/L, and get this mother liquor 7.8mL-62.2mL in beaker, add water to 500mL, adjust pH is 4; Take cetyl trimethylammonium bromide (CTAB) pressed powder, add water 500mL, and under 40 DEG C of conditions, heating makes it fully dissolve in 1 minute, stirs and makes it be uniformly dispersed;
While stirring cerium salt mother liquor, cetyl trimethylammonium bromide (CTAB) solution is joined in cerium salt mother liquor, continue stirring 20 minutes, mixing solutions is uniformly dispersed, obtain the mixing solutions 1L that cerium solution that concentration is 0.01mol/L ~ 0.08 mol/L and concentration are the CTAB solution of 0.1 g/L ~ 3.0 g/L, the pH value regulating initial mixing solution is 3 ~ 5, is then sealed by beaker mouth with preservative film, pricks several hole;
(2) take 1.2 ~ 3 times that precipitation agent molar weight is corresponding cerium salt molar weight, after weighing up, make it be uniformly dispersed with mortar grinding powder, load in culture dish, with preservative film, culture dish collar extension is sealed simultaneously, prick several hole;
(3) beaker of the cerium salt in moisture eliminator and cetyl trimethylammonium bromide (CTAB) mixing solutions is put into the two-layer up and down of moisture eliminator respectively with the culture dish of dress precipitation agent, react 15 ~ 25 days in moisture eliminator, obtain elliposoidal granular precursor;
(4) elliposoidal granular precursor is through 400 ~ 1000 DEG C of roastings, obtains the cerium oxide particle of micron-order ellipsoidal.
3.
the preparation method of micron-order ellipsoidal cerium oxide as claimed in claim 2, is characterized in that: cerium salt used is water-soluble cerium salt, and described water-soluble cerium salt is cerous nitrate, cerous sulfate, cerous acetate or Cerium II Chloride.
4.
the preparation method of micron-order ellipsoidal cerium oxide as claimed in claim 3, it is characterized in that: described precipitation agent is labile carbonate under the room temperature condition containing carbonate, described is volatile salt or bicarbonate of ammonia containing labile carbonate under the room temperature condition of carbonate.
5.
the preparation method of micron-order ellipsoidal cerium oxide as claimed in claim 4, is characterized in that: react after 15 ~ 25 days in moisture eliminator, replace washing sample three times by dehydrated alcohol and secondary deionized water, at 30-60 DEG C, drying obtains elliposoidal granular precursor.
6.
the preparation method of micron-order ellipsoidal cerium oxide as claimed in claim 5, it is characterized in that: elliposoidal granular precursor 400 ~ 1000 DEG C of roastings, heat-up rate 200 DEG C/h, soaking time 2h, cool to room temperature with the furnace, obtain micron-order ellipsoidal cerium oxide particle.
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