CN103965036B - A kind of preparation method of taper cesium formate - Google Patents
A kind of preparation method of taper cesium formate Download PDFInfo
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- CN103965036B CN103965036B CN201410197833.1A CN201410197833A CN103965036B CN 103965036 B CN103965036 B CN 103965036B CN 201410197833 A CN201410197833 A CN 201410197833A CN 103965036 B CN103965036 B CN 103965036B
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- mixing solutions
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- cesium formate
- taper
- white precipitate
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- 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
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- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract
The invention provides a kind of preparation method of taper cesium formate, the present invention is by the following technical solutions: the ethylene glycol of measured amounts is poured in three neck round-bottomed flasks, add a certain amount of solubility cerium salt, and then a certain amount of PEG-4000 is added 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 back flow reaction certain hour, can obtain homogeneous milk shape solution.White precipitate is centrifugal, washing, is then placed in 100 DEG C of dry 12h of baking oven and obtains white cesium 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 prepares taper cesium formate.
Background technology
Cesium formate is a kind of important rare earth compound, the peculiar optical property caused due to the special 4f electronic shell of its inside and chemical property, being subject to the extensive concern of material circle and being applied to many fields, is the important persursor material that synthesis has special appearance cerium dioxide.Therefore, the ceria material that the cesium formate material that Design and manufacture has different-shape has its identical pattern for synthesis has important meaningful, is also the research field become 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, its product good uniformity prepared, good crystallinity, and be easy to batch production.
The present invention is by the following technical solutions:
The ethylene glycol of measured amounts is poured in three neck round-bottomed flasks, adds 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 homogeneous milk shape emulsion.White precipitate is centrifugal, washing, is then placed in 100 DEG C of dry 12h of baking oven and obtains white cesium formate powder.
Described preparation method, the solvent described in it is ethylene glycol and PEG-4000, and its volume is respectively 20-90mL and 10-30mL.
Described preparation method, the solubility cerium salt described in it is ceric ammonium nitrate, and 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 easily controls, safe and reliable, economical convenient and be easy to amplify and the advantage such as suitability for industrialized production; Gained taper cesium formate pattern and dimensional homogeneity good, the advantages such as starting material are cheap and easy to get.
Accompanying drawing explanation
X-ray diffraction (XRD) collection of illustrative plates that Fig. 1 is product shown in embodiment 1;
Scanning power shovel (SEM) the pattern photo that Fig. 2 is product shown in embodiment 1;
Embodiment
Embodiment 1
First measure 30mL ethylene glycol to 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 of backflow, 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 homogeneous milk shape solution.After white precipitate is centrifugal, rinse 3 times respectively with dehydrated alcohol and deionized water water, be then placed in 100 DEG C of dry 12h of baking oven and obtain white powder.
Embodiment 2
First measure 30mL ethylene glycol to 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 of backflow, 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 homogeneous milk shape solution.After white precipitate is centrifugal, rinse 3 times respectively with dehydrated alcohol and deionized water water, be then placed in 100 DEG C of dry 12h of baking oven and obtain white powder.
Embodiment 3
First measure 60mL ethylene glycol to 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 of backflow, 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 homogeneous milk shape solution.After white precipitate is centrifugal, rinse 3 times respectively with dehydrated alcohol and deionized water water, be then placed in 100 DEG C of dry 12h of baking oven and obtain white powder.
From the test result of the taper cesium formate XRD that the present invention obtains, the cesium formate characteristic diffraction peak that the present invention obtains is cesium formate crystalline phase.Scanning electron microscope (SEM) pattern photo shows that the cesium formate that the present invention obtains is taper.
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (4)
1. the preparation method of a taper cesium formate, operation steps is as follows: the ethylene glycol of measured amounts is poured in three neck round-bottomed flasks, add a certain amount of solubility cerium salt, described solubility cerium salt is ceric ammonium nitrate, and then a certain amount of PEG-4000 is added 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 2h, start to occur milky white precipitate, after reaction certain hour, homogeneous milk shape solution can be obtained, white precipitate is centrifugal, washing, is then placed in 100 DEG C of dry 12h of baking oven and obtains white cesium formate powder.
2. preparation method according to claim 1, is characterized in that ethylene glycol and PEG-4000 volume are respectively 20-90mL and 10-30mL.
3. preparation method according to claim 1, it 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, it 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 |
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| CN201410197833.1A CN103965036B (en) | 2014-05-12 | 2014-05-12 | A kind of preparation method of taper cesium formate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410197833.1A CN103965036B (en) | 2014-05-12 | 2014-05-12 | A kind of preparation method of taper cesium formate |
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| CN103965036A CN103965036A (en) | 2014-08-06 |
| CN103965036B true CN103965036B (en) | 2015-09-16 |
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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 |
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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.》.2013,第52卷11734-11743. * |
| Lei He,et.al.Solvothermal synthesis and characterization of ceria with solid and hollow spherical and multilayered morphologies.《Applied Surface Science》.2014,第332卷147-154. * |
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