CN1312044C - Process for synthesizing nano cerium oxide crystal material - Google Patents
Process for synthesizing nano cerium oxide crystal material Download PDFInfo
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- CN1312044C CN1312044C CNB2005100122029A CN200510012202A CN1312044C CN 1312044 C CN1312044 C CN 1312044C CN B2005100122029 A CNB2005100122029 A CN B2005100122029A CN 200510012202 A CN200510012202 A CN 200510012202A CN 1312044 C CN1312044 C CN 1312044C
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- cerium oxide
- cerium
- crystal material
- oxide crystal
- melting salt
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- 239000013078 crystal Substances 0.000 title claims abstract description 26
- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 23
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims abstract description 13
- 230000002194 synthesizing effect Effects 0.000 title abstract 3
- 150000003839 salts Chemical class 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 11
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 4
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims abstract 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 33
- 238000001816 cooling Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- 238000010189 synthetic method Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical group OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 2
- 235000010333 potassium nitrate Nutrition 0.000 claims description 2
- 239000004323 potassium nitrate Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 150000001785 cerium compounds Chemical class 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 description 11
- 238000001914 filtration Methods 0.000 description 10
- 206010013786 Dry skin Diseases 0.000 description 9
- 238000001035 drying Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 238000010792 warming Methods 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 7
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 235000011868 grain product Nutrition 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to a method for synthesizing a nanometer cerium oxide crystal material, which belongs to the technical field of the synthesis technique of inorganic material or a catalytic agent. The present invention adopts easy-decomposition cerium compound as precursor, and the precursor is mixed homogeneously with molten salt according to the mole ratio of cerium to the molten salt as 1: 1 to 1: 9; then, the mixture is heated to a temperature higher than the melting point of the added molten salt and lower than 950 DEG C, and then calcination at the constant temperature is carried out; finally, product after the reaction is cooled and washed for removing the residual molten salt, and the product after the reaction is dried under normal pressure or vacuum with the temperature of 50 to 300 DEG C to obtain the nanometer cerium oxide crystal material. The present invention has the advantage of simple process; in addition, by controlling different synthesizing conditions, the grain size of the nanometer cerium oxide can be controlled effectively, and different requirements to the grain size under different application conditions can be satisfied.
Description
Invention field
The present invention relates to preparation of nanomaterials, particularly the synthetic method of nano cerium oxide crystal material belongs to inorganic materials synthetic technology or catalyzer synthesis technical field.
Background technology
Cerium oxide has appraising at the current rate of uniqueness and stores up the oxygen performance, can be widely used in aspects such as auto-exhaust catalyst, fuel cell, luminescent material, uv-absorbing material, electronic ceramics, polishing powder.
The granularity of cerium oxide and surface properties are very huge to its performance impact.Nano-cerium oxide can effectively improve support strength as catalyst adjuvant, improves the stability of catalyzer, and storage oxygen performance is obvious; And cerium oxide is when being applied in the polishing field, and its granularity is more little, and it is high more then to polish fineness.Therefore developing nano oxidized cerium crystal has important practical value.
Someone has studied as the synthetic cerium oxide nano materials of wet chemical methods such as solid phase method and the precipitator method, sol-gel method, hydrothermal method, microemulsion method or spray heating decomposition.Relative molten-salt growth method, these methods exist reagent cost higher (as microemulsion method), equipment requirements complexity (as spray heating decomposition) or reunite serious (as the precipitator method) etc. not enough, and the granularity of gained material is difficult for being regulated and control; Hydrothermal method can access the uniform material of composition, but output is less, is difficult in industrial enforcement.
Summary of the invention
The objective of the invention is deficiency, provide a kind of working condition and technology simple, product granularity preparation method little and even, that also can be controlled at existing synthetic method.
Above-mentioned purpose is achieved by the following scheme:
A kind of synthetic method of nano cerium oxide crystal material is characterized in that this method carries out as follows:
1) be precursor with the easy decomposition compound of cerium, 1: 1～9 mixed in molar ratio are even to press cerium and melting salt or potassium hydroxide, miscellany is heated to the melting salt that added or more than the potassium hydroxide fusing point to 950 ℃, constant temperature calcining 0.5～24 hour under this temperature then; The easy decomposition compound of described cerium is oxalate, carbonate, acetate or the oxyhydroxide of different valence state cerium; Described melting salt adopts at least a in saltpetre, Repone K, the Potassium ethanoate;
2) with reacted product cooling, remaining melting salt or potassium hydroxide are removed in washing, dry under normal pressure or vacuum then, and bake out temperature is 50～300 ℃, obtains nano cerium oxide crystal material.
Heat-up rate when miscellany heats is 1～100 ℃/min, and the cooling rate during the product cooling is 1～200 ℃/min.
The melting salt of flush away remnants adopts at least a in water, acetonitrile, ethanol or the propyl carbinol.
The present invention compared with prior art; have the following advantages and the high-lighting effect: the present invention has kept the simple advantage of solid-phase process preparation; and by adding different melting salts or potassium hydroxide; the liquid environment that provides for reaction; be beneficial to promptly that reaction is all even to be carried out rapidly; between nano-cerium oxide crystal grain product, constitute simultaneously liquid protection environment, hindered the crystal grain reunion.Adopt synthetic method of the present invention, can obtain near the nano oxidized cerium crystal of globular, by the control synthesis condition, the grain-size of cerium oxide can change within the scope of 5～150nm, can satisfy the requirement of the crystal size under the different application condition.
Description of drawings
Fig. 1: the nano-cerium oxide X-ray diffraction in crystals collection of illustrative plates (embodiment 1) that the present invention is prepared.
Fig. 2: the nano-cerium oxide crystalline transmission electron microscope photo (embodiment 2) that the present invention is prepared.
Fig. 3: the nano-cerium oxide crystalline transmission electron microscope photo (embodiment 3) that the present invention is prepared.
Fig. 4: the nano-cerium oxide crystalline transmission electron microscope photo (embodiment 4) that the present invention is prepared.
Fig. 5: the nano-cerium oxide crystalline transmission electron microscope photo (embodiment 5) that the present invention is prepared.
Fig. 6: the nano-cerium oxide X-ray diffraction in crystals collection of illustrative plates (embodiment 6) that the present invention is prepared.
Embodiment
Adopt the product of the present invention's preparation, the material crystals structure adopts X-ray diffraction method to measure, and surface topography is by determination of transmission electron microscopy, with N
2Gas physical adsorption BET method is measured specific surface.
Embodiment 1
With Ce (NO
3)
36H
2O and K
2C
2O
4H
2O is a raw material, and liquid-phase mixing is reacted and obtained Ce
2(C
2O
4)
3Precipitation, dry 12h in 80～90 ℃ of baking ovens; Press Ce:KNO
31: 3 ratio of mol ratio adds quantitative KNO in precipitation
3, fully ground and mixed is even, is warming up to 500 ℃ with 5 ℃/min speed, constant temperature calcining 3h, and then with the stove naturally cooling, roasting 3h under differing temps with deionized water thorough washing, filtration, 130 ℃ of following thorough dryings, obtains the nano Ce O that particle diameter is about 10nm
2Crystal.
Embodiment 2
With Ce (NO
3)
36H
2O and K
2C
2O
3H
2O is a raw material, and liquid-phase mixing is reacted and obtained Ce
2(C
2O
4)
3Precipitation, dry 6h in 120 ℃ of baking ovens; Press Ce:KNO
31: 3 ratio of mol ratio adds quantitative KNO in precipitation
3, fully ground and mixed is even, is warming up to 600 ℃ with 10 ℃/min speed, and constant temperature calcining 3h then with the cooling of 20 ℃/min speed, with deionized water and ethanol thorough washing, filtration, 200 ℃ of following thorough dryings, obtains the nano Ce O that particle diameter is about 20nm
2Crystal.
Embodiment 3
With Ce (NO
3)
36H
2O and K
2C
2O
4H
2O solution mixes, and reaction obtains Ce
2(C
2O
4)
3Precipitation, dry 5h in 150 ℃ of baking ovens; Press Ce: KNO
31: 3 ratio of mol ratio adds quantitative KNO in precipitation
3, fully ground and mixed is even, is warming up to 700 ℃ with 25 ℃/min speed, and constant temperature calcining 3h then with the cooling of 40 ℃/min speed, with deionized water and acetonitrile thorough washing, filtration, 60～80 ℃ of following thorough dryings, obtains the nano Ce O that particle diameter is about 50nm
2Crystal.
Embodiment 4
With Ce (NO
3)
36H
2O and K
2C
2O
4H
2O solution hybrid reaction obtains Ce
2(C
2O
4)
3Precipitation, dry 24h in 60 ℃ of baking ovens; Press Ce: KNO
31: 3 ratio of mol ratio adds quantitative KNO
3, fully grinding is mixed, and is warming up to 800 ℃ with 50 ℃/min speed, and constant temperature calcining 3h with the cooling of 80 ℃/min speed, with propyl carbinol thorough washing, filtration, 60～80 ℃ of following thorough dryings, obtains the nano Ce O that particle diameter is about 100nm then
2Crystal.
Embodiment 5
With KCl is fused salt, and in Ce: 1: 5 ratio of KCl mol ratio is at Ce
2(C
2O
4)
3Add quantitative KCl, fully grinding is mixed, and is warming up to 850 ℃ with 40 ℃/min speed, constant temperature calcining 3h is then with 10 ℃/min speed cooling, with propyl carbinol and deionized water thorough washing, filtration, 60～80 ℃ of following thorough dryings, obtain the CeO that particle diameter is about 80nm
2Crystal.
Embodiment 6
With Ce (NO
3)
36H
2O and K
2CO
3Be raw material, liquid phase reaction obtains Ce
2(CO
3)
3Precipitation; Press Ce: KNO
31: 3 ratio of mol ratio adds quantitative KNO in precipitation
3, fully ground and mixed is even, is warming up to 600 ℃ with 5 ℃/min speed, and constant temperature calcining 1h and 9h respectively with ethanol thorough washing, filtration, 90 ℃ of following thorough dryings, obtain particle diameter and are about 14 and the nano Ce O of 22nm
2Crystal.
Embodiment 7
In Ce: 1: 9 ratio of KCl mol ratio is at Ce
2(C
2O
4)
3Add quantitative KCl, fully grinding is mixed, and is warming up to 850 ℃ with 20 ℃/min speed, constant temperature calcining 3h, and cooling naturally with ethanol thorough washing, filtration, 250 ℃ of following thorough dryings, obtains the CeO that particle diameter is about 83nm then
2Crystal.
Embodiment 8
Press Ce: KNO
31: 1 ratio of mol ratio is at Ce
2(C
2O
4)
3Add quantitative KNO
3, fully grinding is mixed, and is warming up to 600 ℃ with 10 ℃/min speed, constant temperature calcining 3h, and cooling naturally with deionized water thorough washing, filtration, 100 ℃ of following thorough dryings, obtains the CeO that particle diameter is about 22nm then
2Crystal.
Embodiment 9
Under heating condition with commercially available common CeO
2Powder dissolution dropwise adds the KOH solution of 1mol/L under the vigorous stirring in salpeter solution, obtain Ce (OH)
4Precipitation fully continues to stir ageing 5h in the back to precipitation, and with sedimentation and filtration, washing back dry 8h under 110 ℃ of temperature, in Ce: 1: 5 ratio of KOH mol ratio is at Ce (OH)
4Add quantitative KOH, fully grind and be mixed, be warming up to 650 ℃ with 10 ℃/min speed, constant temperature calcining 3h lowers the temperature then naturally, with ethanol and deionized water thorough washing, filtration, 120 ℃ of following thorough dryings, obtains the CeO that particle diameter is about 15nm
2Crystal.
Claims (3)
1. the synthetic method of a nano cerium oxide crystal material is characterized in that this method carries out as follows:
1) be precursor with the easy decomposition compound of cerium, 1: 1～9 mixed in molar ratio are even to press cerium and melting salt or potassium hydroxide, miscellany is heated to the melting salt that added or more than the potassium hydroxide fusing point to 950 ℃, constant temperature calcining 0.5～24 hour under this temperature then; The easy decomposition compound of described cerium is oxalate, carbonate, acetate or the oxyhydroxide of different valence state cerium; Described melting salt adopts at least a in saltpetre, Repone K, the Potassium ethanoate,
2) with reacted product cooling, remaining melting salt or potassium hydroxide are removed in washing, dry under normal pressure or vacuum then, and bake out temperature is 50～300 ℃, obtains nano cerium oxide crystal material.
2. according to the described synthetic method of claim 1, it is characterized in that: step 2) melting salt of described flush away remnants or potassium hydroxide adopts at least a washing in water, acetonitrile, ethanol or the propyl carbinol.
3. according to claim 1 or 2 described synthetic methods, it is characterized in that: the heat-up rate in miscellany when heating is 1～100 ℃/min in the step 1), step 2) in cooling rate during the product cooling be 1～200 ℃/min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100122029A CN1312044C (en) | 2005-07-15 | 2005-07-15 | Process for synthesizing nano cerium oxide crystal material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100122029A CN1312044C (en) | 2005-07-15 | 2005-07-15 | Process for synthesizing nano cerium oxide crystal material |
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|---|---|
| CN1724380A CN1724380A (en) | 2006-01-25 |
| CN1312044C true CN1312044C (en) | 2007-04-25 |
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|---|---|---|---|
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111099650A (en) * | 2020-01-21 | 2020-05-05 | 江苏理工学院 | CeO2Molten salt method for synthesizing nano spherical particles |
| CN112028105B (en) * | 2020-08-06 | 2023-09-05 | 常州市卓群纳米新材料有限公司 | Method for preparing nano praseodymium oxide by fused salt coprecipitation method |
| CN113044873A (en) * | 2021-04-16 | 2021-06-29 | 陕西科技大学 | CeO for chemical mechanical polishing2Nanoparticles and method for preparing same |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1426963A (en) * | 2001-12-17 | 2003-07-02 | 暨南大学 | Manufacturing method of nano cerium oxide powder |
| CN1522228A (en) * | 2002-04-15 | 2004-08-18 | LG��ѧ��ʽ���� | Preparation of single crystalline cerium oxide powder |
| CN1532147A (en) * | 2003-03-21 | 2004-09-29 | 中国科学院生态环境研究中心 | Process for preparing nano cerium dioxide |
| CN1556039A (en) * | 2004-01-09 | 2004-12-22 | 山东师范大学 | Synthesis method of cerium oxide nano material |
-
2005
- 2005-07-15 CN CNB2005100122029A patent/CN1312044C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1426963A (en) * | 2001-12-17 | 2003-07-02 | 暨南大学 | Manufacturing method of nano cerium oxide powder |
| CN1522228A (en) * | 2002-04-15 | 2004-08-18 | LG��ѧ��ʽ���� | Preparation of single crystalline cerium oxide powder |
| CN1532147A (en) * | 2003-03-21 | 2004-09-29 | 中国科学院生态环境研究中心 | Process for preparing nano cerium dioxide |
| CN1556039A (en) * | 2004-01-09 | 2004-12-22 | 山东师范大学 | Synthesis method of cerium oxide nano material |
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