CN103965036A - Method for preparing tapered cerium formate - Google Patents
Method for preparing tapered cerium formate Download PDFInfo
- Publication number
- CN103965036A CN103965036A CN201410197833.1A CN201410197833A CN103965036A CN 103965036 A CN103965036 A CN 103965036A CN 201410197833 A CN201410197833 A CN 201410197833A CN 103965036 A CN103965036 A CN 103965036A
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- CN
- China
- Prior art keywords
- certain amount
- preparation
- mixing solutions
- white
- mixed solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 238000000034 method Methods 0.000 title abstract description 7
- UADULFIZHZKEOP-UHFFFAOYSA-K cerium(3+);triformate Chemical compound [Ce+3].[O-]C=O.[O-]C=O.[O-]C=O UADULFIZHZKEOP-UHFFFAOYSA-K 0.000 title abstract 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002244 precipitate Substances 0.000 claims abstract description 11
- 238000010992 reflux Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 6
- 150000000703 Cerium Chemical class 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 3
- ATZQZZAXOPPAAQ-UHFFFAOYSA-M caesium formate Chemical compound [Cs+].[O-]C=O ATZQZZAXOPPAAQ-UHFFFAOYSA-M 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical group [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 claims description 10
- 229920001030 Polyethylene Glycol 4000 Polymers 0.000 claims description 7
- 239000008267 milk Substances 0.000 claims description 5
- 210000004080 milk Anatomy 0.000 claims description 5
- 235000013336 milk Nutrition 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 abstract 4
- 239000000243 solution Substances 0.000 abstract 2
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003321 amplification Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- -1 rare earth compound Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention provides a method for preparing tapered cerium formate. According to the following technical scheme, the method disclosed by the invention comprises the steps of: measuring and pouring a certain amount of ethylene glycol into a three-necked round bottom flask, adding a certain amount of soluble cerium salt to obtain a mixed solution, then adding a certain amount of polyethylene glycol-400 into the mixed solution again, stirring until the mixed solution is colorless and transparent, and heating and refluxing the mixed solution, wherein the colorless and transparent solution becomes yellow-brown at the beginning of heating, white precipitate begins to appear after about 2 hours, and a uniform milky solution can be obtained after the reflux reaction is carried out for a period of time; centrifuging the white precipitate, washing and then drying in an oven of which the temperature is 100 DEG C for 12 hours to obtain white cerium formate powder.
Description
Technical field
The present invention relates to a kind of preparation method of taper cesium formate, be specifically related to a kind of method that circumfluence method is prepared taper cesium formate.
Background technology
Cesium formate is a kind of important rare earth compound, the peculiar optical property and the chemical property that cause due to the special 4f electronic shell of its inside, being subject to the extensive concern of material circle and being applied to many fields, is the synthetic important persursor material with special appearance cerium dioxide.Therefore, the cesium formate material that Design and manufacture has a different-shape has important meaningful for the synthetic cerium dioxide material with its identical pattern, be also the research field becoming more and more important in Materials science forward position.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of taper cesium formate, the product good uniformity that it is prepared, good crystallinity, and be easy to batch production.
The present invention is by the following technical solutions:
Measure a certain amount of ethylene glycol and pour in three neck round-bottomed flasks, add a certain amount of solubility cerium salt, and then add a certain amount of PEG-4000 in above-mentioned mixing solutions, above-mentioned mixing solutions is stirred to water white transparency.This mixing solutions of reflux, can find, colourless transparent solution has just started to become yellowish brown in heating, after about 2h, starts to occur milky white precipitate, after backflow certain hour, can obtain the milk shape emulsion of homogeneous.By centrifugal white precipitate, washing, be then placed in the dry 12h of 100 DEG C of baking ovens and obtain white cesium formate powder.
Described preparation method, the solvent described in it is ethylene glycol and PEG-4000, its volume is respectively 20-90mL and 10-30mL.
Described preparation method, the solubility cerium salt described in it is ceric ammonium nitrate, its concentration is 0.05-0.25mol/L.
Described preparation method, described reflux temperature is between 160～180 DEG C, and return time is between 16-36h.
Product Process involved in the present invention is simple and easy to realize, and constant product quality and process repeatability can be good, and reaction parameter is easily controlled, safe and reliable, economy is convenient and be easy to the advantages such as amplification and suitability for industrialized production; The advantages such as gained taper cesium formate pattern and dimensional homogeneity are good, and starting material are cheap and easy to get.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of product shown in embodiment 1;
Fig. 2 is scanning power shovel (SEM) the pattern photo of product shown in embodiment 1;
Embodiment
Embodiment 1
First measure 30mL ethylene glycol and pour in three neck round-bottomed flasks, add 2.74g (5mmol) ceric ammonium nitrate, and then add 10mL PEG-4000 in above-mentioned mixing solutions, above-mentioned mixing solutions is stirred to water white transparency.Be heated to 160 DEG C of these mixing solutionss that reflux, can find, colourless transparent solution has just started to become yellowish brown in heating, after about 2h, starts to occur milky white precipitate, after back flow reaction 24h, can obtain the milk shape solution of homogeneous.After white precipitate is centrifugal, rinse respectively 3 times with dehydrated alcohol and deionized water water, be then placed in the dry 12h of 100 DEG C of baking ovens and obtain white powder.
Embodiment 2
First measure 30mL ethylene glycol and pour in three neck round-bottomed flasks, add 4.11g (7.5mmol) ceric ammonium nitrate, and then add 10mL PEG-4000 in above-mentioned mixing solutions, above-mentioned mixing solutions is stirred to water white transparency.Be heated to 160 DEG C of these mixing solutionss that reflux, can find, colourless transparent solution has just started to become yellowish brown in heating, after about 2h, starts to occur milky white precipitate, after back flow reaction 18h, can obtain the milk shape solution of homogeneous.After white precipitate is centrifugal, rinse respectively 3 times with dehydrated alcohol and deionized water water, be then placed in the dry 12h of 100 DEG C of baking ovens and obtain white powder.
Embodiment 3
First measure 60mL ethylene glycol and pour in three neck round-bottomed flasks, add 2.74g (5mmol) ceric ammonium nitrate, and then add 20mL PEG-4000 in above-mentioned mixing solutions, above-mentioned mixing solutions is stirred to water white transparency.Be heated to 160 DEG C of these mixing solutionss that reflux, can find, colourless transparent solution has just started to become yellowish brown in heating, after about 2h, starts to occur milky white precipitate, after back flow reaction 24h, can obtain the milk shape solution of homogeneous.After white precipitate is centrifugal, rinse respectively 3 times with dehydrated alcohol and deionized water water, be then placed in the dry 12h of 100 DEG C of baking ovens and obtain white powder.
The test result of the taper cesium formate XRD making from the present invention, the cesium formate characteristic diffraction peak that the present invention makes is cesium formate crystalline phase.Scanning electron microscope (SEM) pattern photo shows that the cesium formate that the present invention makes is taper.
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (4)
1. measure a certain amount of ethylene glycol and pour in three neck round-bottomed flasks, add a certain amount of solubility cerium salt, and then add a certain amount of PEG-4000 in above-mentioned mixing solutions, above-mentioned mixing solutions is stirred to water white transparency.This mixing solutions of reflux, can find, colourless transparent solution has just started to become yellowish brown in heating, after about 2h, starts to occur milky white precipitate, after reaction certain hour, can obtain the milk shape solution of homogeneous.By centrifugal through precipitating white, washing, be then placed in the dry 12h of 100 DEG C of baking ovens and obtain white cesium formate powder.
2. preparation method according to claim 1, described preparation method, is characterized in that described solvent is ethylene glycol and PEG-4000, its volume is respectively 20-90mL and 10-30mL.
3. preparation method according to claim 1, described preparation method, is characterized in that described solubility cerium salt is ceric ammonium nitrate, its concentration is 0.05-0.25mol/L.
4. preparation method according to claim 1, described preparation method, is characterized in that described reflux temperature is between 160～180 DEG C, return time is between 16-36h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410197833.1A CN103965036B (en) | 2014-05-12 | 2014-05-12 | A kind of preparation method of taper cesium formate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410197833.1A CN103965036B (en) | 2014-05-12 | 2014-05-12 | A kind of preparation method of taper cesium formate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103965036A true CN103965036A (en) | 2014-08-06 |
| CN103965036B CN103965036B (en) | 2015-09-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410197833.1A Expired - Fee Related CN103965036B (en) | 2014-05-12 | 2014-05-12 | A kind of preparation method of taper cesium formate |
Country Status (1)
| Country | Link |
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| CN (1) | CN103965036B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100486959B1 (en) * | 2003-01-29 | 2005-05-03 | 한국화학연구원 | Preparation method of ceria particles with nano-size |
| CN101117233A (en) * | 2007-07-23 | 2008-02-06 | 北京科技大学 | Method for preparing high specific surface area meso-porous cerium dioxide micro-balloon |
| CN101792171A (en) * | 2010-03-04 | 2010-08-04 | 上海大学 | Preparation method of cerium oxide nanoballs |
-
2014
- 2014-05-12 CN CN201410197833.1A patent/CN103965036B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100486959B1 (en) * | 2003-01-29 | 2005-05-03 | 한국화학연구원 | Preparation method of ceria particles with nano-size |
| CN101117233A (en) * | 2007-07-23 | 2008-02-06 | 北京科技大学 | Method for preparing high specific surface area meso-porous cerium dioxide micro-balloon |
| CN101792171A (en) * | 2010-03-04 | 2010-08-04 | 上海大学 | Preparation method of cerium oxide nanoballs |
Non-Patent Citations (2)
| Title |
|---|
| CHRISTOPH HENNIG，ET.AL: "Crystal Structure and Solution Species of Ce(III) and Ce(IV) Formates:From Mononuclear to Hexanuclear Complexes", 《INORG. CHEM.》, vol. 52, 2013, pages 11734 - 11743 * |
| LEI HE，ET.AL: "Solvothermal synthesis and characterization of ceria with solid and hollow spherical and multilayered morphologies", 《APPLIED SURFACE SCIENCE》, vol. 332, 24 October 2014 (2014-10-24), pages 147 - 154 * |
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| Publication number | Publication date |
|---|---|
| CN103965036B (en) | 2015-09-16 |
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Granted publication date: 20150916 Termination date: 20200512 |