CN107529519B - A kind of yolk-shell structure CrF3·3H2The preparation method of O - Google Patents
A kind of yolk-shell structure CrF3·3H2The preparation method of O Download PDFInfo
- Publication number
- CN107529519B CN107529519B CN201710946633.5A CN201710946633A CN107529519B CN 107529519 B CN107529519 B CN 107529519B CN 201710946633 A CN201710946633 A CN 201710946633A CN 107529519 B CN107529519 B CN 107529519B
- Authority
- CN
- China
- Prior art keywords
- yolk
- shell structure
- minutes
- crcl
- crf
- 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.)
- Active
Links
Abstract
A kind of yolk-shell structure CrF3·3H2The preparation method of O belongs to function nano Material Field.Present invention process process are as follows: 1. by CrCl3·6H2O、KF·2H2O is made into microemulsion with surfactant, cosurfactant, octane, deionized water respectively according to a certain percentage；2. two kinds of microemulsions of configuration are carried out ultrasound, the time is 5~30 minutes, continues stirring 5~30 minutes KF2H2O solution is added to CrCl3·6H2It is reacted in O, the reaction time is 5~120 minutes, this process stirs always；3. the mixed solution of chloroform and methanol is added after the reaction was completed, the green precipitate generated in beaker obtains yolk-shell structure CrF after being centrifuged, cleaning3·3H2O spheric granules.The present invention can prepare yolk-shell structure CrF by controlling reaction condition3·3H2O spheric granules, simple process, method is novel, and with short production cycle, powder dispersibility is good, being capable of large-scale promotion.
Description
Technical field
The invention belongs to function nano Material Fields, and in particular to a kind of yolk-shell structure CrF3·3H2The preparation side of O
Method.
Background technique
Into after 21 century, environmental problem and energy crisis become the problem of mankind face jointly.In order to be asked in face of these
Topic, finds the approach of sustainable development, and attention of the development and utilization of the renewable sources of energy increasingly by various countries is chargeable secondary
Battery has also obtained significant progress.Lithium ion battery has high-energy density, high power density, has extended cycle life, work electricity
The advantages that pressing big high and operating temperature range, memory-less effect and having a safety feature has obtained wide in portable
General application.The performance of battery material plays conclusive effect for the development of battery.Therefore, stable structure, price are found just
Suitable and energy large-scale application battery material is the developing direction of current field of lithium ion battery.
Charomic fluoride and its hydrate are a kind of important chromic salts, are widely used as the mordant dyeing of the mothproofing agent, wool of fabric
Agent, industrial disinfection agent, marmorean colorant, metal polish etc..Since charomic fluoride and its hydrate have and can accommodate
The crystal structure of a large amount of lithium ions insertions, in recent years, researcher charomic fluoride and its hydrate research sight turned to lithium from
Sub- field of batteries starts to prepare charomic fluoride and its hydrate using different methods.Usual charomic fluoride is by flow of hydrogen fluoride
The method preparation of chromium chloride is heated, this method condition is harsh, device is special, equipment seriously corroded, working environment are severe.Charomic fluoride
And its hydrate still suffers from the problems such as preparation is difficult, and pattern is irregular.Control synthesizes specific morphology and high-specific surface area
Charomic fluoride and its hydrate, for charomic fluoride nano material field of batteries it is further development have great importance.Just
For literature survey, the charomic fluoride and its hydrate prepared at present are mainly irregular particle, have no yolk-shell structure
CrF3·3H2O report.
Summary of the invention
The present invention provide it is a kind of simple, efficiently, low cost prepare yolk-shell structure CrF3·3H2The preparation method of O.
A kind of yolk-shell structure CrF3·3H2The preparation method of O, it is characterised in that include the following steps:
1) by CrCl3·6H2O、KF·2H2O is pressed with surfactant, cosurfactant, octane, deionized water respectively
It is made into microemulsion according to certain ratio, wherein CrCl3·6H2O and KF2H2The molar ratio of O is 1:(2~5), CrCl3·6H2O
Mass ratio with surfactant, cosurfactant, octane, deionized water is 1:(2~6): 5:22:3；
2) two kinds of microemulsions of configuration are subjected to ultrasound, the time is 5~30 minutes, continues stirring 5~30 minutes KF
2H2O solution is added to CrCl3·6H2It is reacted in O, the reaction time is 5~120 minutes, this process stirs always；
3) be added the mixed solution of chloroform and methanol after the reaction was completed, the green precipitate generated in container pass through from
Yolk-shell structure CrF is obtained after the heart, cleaning3·3H2The spheric granules of O, wherein the volume ratio of chloroform and methanol be (1~
3): 1.
Surfactant described in step 1) is CTAB, and cosurfactant is n-butanol, and octane is normal octane or different pungent
Alkane, octane quality score is 96~99%.
Solution used in cleaning described in step 3) is methanol, deionized water and ethyl alcohol, and cleaning sequence is first methanol, followed by
Deionized water finally uses ethyl alcohol.
Yolk described in step 3)-shell structure CrF3·3H2The partial size of O particle is 100nm~5 μm.
A kind of yolk-shell structure CrF proposed by the invention3·3H2The preparation method of O, there is not yet document and other aspects
Report.Preparation method is simple, and the reaction time is short, and cost of material is low.And yolk-shell structure CrF3·3H2O nano particle is due to it
With special structure and lesser size, its specific surface area can be greatly improved, is hopeful it in lithium ion battery and its
Its new ion battery field is widely used.
This method has the advantage that
1) present invention has directly prepared the CrF of novel yolk-shell structure using a step microemulsion method3·3H2O particle.
Method is simple, easily operated, can be completed in room temperature.
2) by the accurate control to reaction time and reacted constituent, different-shape is prepared in a relatively short period of time, no
With the CrF of size3·3H2O particle.
3) the technological reaction process can be controlled accurately, at low cost, be suitble to scale industrial production.
Detailed description of the invention
Fig. 1 is yolk prepared by the present invention-shell structure CrF3·3H2The XRD spectrum of O particle；
Fig. 2 is yolk prepared by the present invention-shell structure CrF3·3H2The FESEM photo of O particle；
Fig. 3 is yolk prepared by the present invention-shell structure CrF3·3H2The TEM photo of O particle.
Specific embodiment
Embodiment one
Weigh CrCl3·6H2O powder 0.5g, KF2H2O powder 0.53g is gone with normal octane 11g, n-butanol 2.5g respectively
Ionized water 1.5ml, CTAB powder 3g forms mixed solution.Two kinds of microemulsions of configuration are subjected to ultrasound, the time is 10 minutes, so
After continue stirring after twenty minutes KF2H2O solution is added to CrCl3·6H2It is reacted in O, the reaction time is 5 minutes,
This process stirs always.Mixed solution (wherein chloroform and the methanol volume of chloroform and methanol are added after the reaction was completed
Than being equal to 1), green precipitate generation is hereafter had in beaker, yolk-shell structure CrF is obtained after being centrifuged, cleaning3·3H2O
Spheric granules.
Embodiment two
Weigh CrCl3·6H2O powder 0.5g, KF2H2O powder 0.53g is gone with normal octane 11g, n-butanol 2.5g respectively
Ionized water 1.5ml, CTAB powder 2g forms mixed solution.Two kinds of microemulsions of configuration are subjected to ultrasound, the time is 10 minutes, so
After continue stirring after twenty minutes KF2H2O solution is added to CrCl3·6H2It is reacted in O, the reaction time is 10 minutes,
This process stirs always.Mixed solution (wherein chloroform and the methanol volume of chloroform and methanol are added after the reaction was completed
Than being equal to 1), green precipitate generation is hereafter had in beaker, yolk-shell structure CrF is obtained after being centrifuged, cleaning3·3H2O
Spheric granules.
Embodiment three
Weigh CrCl3·6H2O powder 0.5g, KF2H2O powder 0.53g is gone with normal octane 11g, n-butanol 2.5g respectively
Ionized water 1.5ml, CTAB powder 2g forms mixed solution.Two kinds of microemulsions of configuration are subjected to ultrasound, the time is 10 minutes, so
After continue stirring after twenty minutes KF2H2O solution is added to CrCl3·6H2It is reacted in O, the reaction time is 20 minutes,
This process stirs always.Mixed solution (wherein chloroform and the methanol volume of chloroform and methanol are added after the reaction was completed
Than being equal to 1), green precipitate generation is hereafter had in beaker, yolk-shell structure CrF is obtained after being centrifuged, cleaning3·3H2O
Spheric granules.
Example IV
Weigh CrCl3·6H2O powder 0.5g, KF2H2O powder 0.53g is gone with normal octane 11g, n-butanol 2.5g respectively
Ionized water 1.5ml, CTAB powder 4g forms mixed solution.Two kinds of microemulsions of configuration are subjected to ultrasound, the time is 10 minutes, so
After continue stirring after ten minutes KF2H2O solution is added to CrCl3·6H2It is reacted in O, the reaction time is 20 minutes,
This process stirs always.Mixed solution (wherein chloroform and the methanol volume of chloroform and methanol are added after the reaction was completed
Than being equal to 2), green precipitate generation is hereafter had in beaker, yolk-shell structure CrF is obtained after being centrifuged, cleaning3·3H2O
Spheric granules.
Embodiment five
Weigh CrCl3·6H2O powder 0.5g, KF2H2O powder 0.53g is gone with normal octane 11g, n-butanol 2.5g respectively
Ionized water 1.5ml, CTAB powder 5g forms mixed solution.Two kinds of microemulsions of configuration are subjected to ultrasound, the time is 10 minutes, so
After continue stirring after twenty minutes KF2H2O solution is added to CrCl3·6H2It is reacted in O, the reaction time is 5 minutes,
This process stirs always.Mixed solution (wherein chloroform and the methanol volume of chloroform and methanol are added after the reaction was completed
Than being equal to 3), green precipitate generation is hereafter had in beaker, yolk-shell structure CrF is obtained after being centrifuged, cleaning3·3H2O's
Spheric granules.
Embodiment six
Weigh CrCl3·6H2O powder 0.5g, KF2H2O powder 0.53g is gone with normal octane 11g, n-butanol 2.5g respectively
Ionized water 1.5ml, CTAB powder 3g forms mixed solution.Two kinds of microemulsions of configuration are subjected to ultrasound, the time is 5 minutes, so
After continue stirring after ten minutes KF2H2O solution is added to CrCl3·6H2It is reacted in O, reaction time 1h, this mistake
Cheng Yizhi stirring.Mixed solution (the wherein chloroform and methanol volume ratio etc. of chloroform and methanol are added after the reaction was completed
It is generated in 1), hereafter having green precipitate in beaker, yolk-shell structure CrF is obtained after being centrifuged, cleaning3·3H2The ball of O
Shape particle.
The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof, the ordinary skill people of fields
Member should be appreciated that can be with modifications or equivalent substitutions are made to specific embodiments of the invention referring to above-described embodiment, these
Without departing from any modification of spirit and scope of the invention or equivalent replacement apply pending claims it
It is interior.
Claims (3)
1. a kind of yolk-shell structure CrF3·3H2The preparation method of O, it is characterised in that include the following steps:
A. by CrCl3·6H2O、KF·2H2O is respectively with surfactant, cosurfactant, octane, deionized water according to one
Fixed ratio is made into microemulsion, wherein CrCl3·6H2O and KF2H2The molar ratio of O is 1:(2~5), CrCl3·6H2O and table
Face activating agent, cosurfactant, octane, deionized water mass ratio be 1:(2~6): 5:22:3；
B. two kinds of microemulsions of configuration are subjected to ultrasound, the time is 5~30 minutes, continues stirring 5~30 minutes KF2H2O is molten
Liquid is added to CrCl3·6H2It is reacted in O, the reaction time is 5~120 minutes, this process stirs always；
C. the mixed solution of chloroform and methanol is added after the reaction was completed, the green precipitate generated in container, which passes through, to be centrifuged, is clear
Yolk-shell structure CrF is obtained after washing3·3H2The spheric granules of O, wherein the volume ratio of chloroform and methanol is (1~3): 1；
Surfactant in the step a is CTAB, and cosurfactant is n-butanol, and octane is normal octane or isooctane,
The mass fraction of octane is 96~99%.
2. yolk according to claim 1-shell structure CrF3·3H2The preparation method of O, it is characterised in that in the step c
Cleaning solution used is methanol, deionized water and ethyl alcohol, and cleaning sequence is first methanol, followed by deionized water, finally uses second
Alcohol.
3. yolk according to claim 1-shell structure CrF3·3H2The preparation method of O, it is characterised in that in the step c
Yolk-shell structure CrF3·3H2The partial size of O particle is 100nm~5 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710946633.5A CN107529519B (en) | 2017-10-12 | 2017-10-12 | A kind of yolk-shell structure CrF3·3H2The preparation method of O |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710946633.5A CN107529519B (en) | 2017-10-12 | 2017-10-12 | A kind of yolk-shell structure CrF3·3H2The preparation method of O |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107529519A CN107529519A (en) | 2018-01-02 |
| CN107529519B true CN107529519B (en) | 2019-04-09 |
Family
ID=60766447
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710946633.5A Active CN107529519B (en) | 2017-10-12 | 2017-10-12 | A kind of yolk-shell structure CrF3·3H2The preparation method of O |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107529519B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1485468A (en) * | 2003-08-13 | 2004-03-31 | 中国科学院长春应用化学研究所 | Process for preparing column shape nanometer barium fluoride crystal |
| CN1923707A (en) * | 2006-09-15 | 2007-03-07 | 重庆大学 | Method of preparing nano tungsten trioxide from microemulsion |
| CN101186815A (en) * | 2007-11-16 | 2008-05-28 | 华中科技大学 | Preparation method for fluorescence metal nano particles |
| CN103466707A (en) * | 2013-08-23 | 2013-12-25 | 甘肃锦世化工有限责任公司 | Production method of chromic chloride hexahydrate |
| CN104192906A (en) * | 2014-08-29 | 2014-12-10 | 四川省银河化学股份有限公司 | Method for preparing chromium trichloride hexahydrate by utilizing sodium chromate |
| CN104250554A (en) * | 2013-06-28 | 2014-12-31 | 长春理工大学 | Neodymium-doped barium fluoride nano powder luminescent material |
-
2017
- 2017-10-12 CN CN201710946633.5A patent/CN107529519B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1485468A (en) * | 2003-08-13 | 2004-03-31 | 中国科学院长春应用化学研究所 | Process for preparing column shape nanometer barium fluoride crystal |
| CN1923707A (en) * | 2006-09-15 | 2007-03-07 | 重庆大学 | Method of preparing nano tungsten trioxide from microemulsion |
| CN101186815A (en) * | 2007-11-16 | 2008-05-28 | 华中科技大学 | Preparation method for fluorescence metal nano particles |
| CN104250554A (en) * | 2013-06-28 | 2014-12-31 | 长春理工大学 | Neodymium-doped barium fluoride nano powder luminescent material |
| CN103466707A (en) * | 2013-08-23 | 2013-12-25 | 甘肃锦世化工有限责任公司 | Production method of chromic chloride hexahydrate |
| CN104192906A (en) * | 2014-08-29 | 2014-12-10 | 四川省银河化学股份有限公司 | Method for preparing chromium trichloride hexahydrate by utilizing sodium chromate |
Non-Patent Citations (1)
| Title |
|---|
| Yolk/shell nanoparticles: classifications, synthesis,properties, and applications;Rahul Purbia等;《Nanoscale》;20151027;第7卷;第19789–19873页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107529519A (en) | 2018-01-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107376958B (en) | NiFeP difunctional transition metal phosphide catalyst and preparation and application thereof | |
| CN106684351B (en) | A kind of nickel-cobalt-manganese ternary presoma and preparation method thereof | |
| CN104167536B (en) | The Preparation method and use of the spherical ferroferric oxide nano granules that size is controlled | |
| CN105140475A (en) | Preparation method of anode material Fe3O4/MoS2 for lithium ion battery | |
| CN107611380A (en) | A kind of preparation method of nickel oxide/stereochemical structure graphene composite material | |
| CN101465420A (en) | Method for preparing nickle lithium manganate material for lithium ion power battery anode | |
| CN107017394B (en) | A kind of pyrophosphoric acid cobalt sodium/carbon graphite alkene anode composite material, preparation and application | |
| CN107082453B (en) | The preparation of hydrated iron barium oxide as water system Magnesium ion battery negative electrode material and application method | |
| CN104971760A (en) | Preparation method of macroporous carbon oxygen reduction catalyst containing sulfur, nitrogen and transition metal element | |
| CN106966438B (en) | A kind of spherical shape Co2AlO4Material and its preparation method and application | |
| CN108588751A (en) | Oxygen application is analysed in chalcogen cobalt-base catalyst, preparation method and electro-catalysis | |
| CN106887608A (en) | The preparation method and application of inexpensive hollow carbon sphere base oxygen reduction catalyst | |
| CN108754534A (en) | A kind of the iron-based non-precious metal catalyst and preparation method of electro-catalysis synthesis ammonia | |
| CN108075181A (en) | A kind of solid-state or colloidal state water-system alkali metal ion battery and preparation method thereof | |
| CN105206832B (en) | A kind of sintering preparation method of zinc load material | |
| CN108232187B (en) | High-dispersion hexagonal nanosheet structure nickel-cobalt-manganese ternary cathode material and preparation method thereof | |
| CN103172126B (en) | A kind of continuity method prepares the method for spherical nickel-cobalt aluminium solid solution ternary material | |
| CN103066249B (en) | Cobalt-based complex oxide/graphene composite material as well as preparation method and application thereof | |
| CN108977676B (en) | A kind of 3R type AB4Hydrogen bearing alloy and its preparation method and application | |
| CN107529519B (en) | A kind of yolk-shell structure CrF3·3H2The preparation method of O | |
| CN103464211A (en) | Preparation method of MnOx/C-PTFE (polytetrafluoroethylene) catalyst pasty fluid | |
| CN105970031B (en) | A kind of hydrolytic hydrogen production aluminium alloy and preparation method thereof | |
| CN109734134B (en) | Preparation and application of coral-like structure ferroferric oxide nano material | |
| CN104362291B (en) | A kind of lithium-enriched cathodic material of lithium ion battery and preparation method thereof and lithium ion battery | |
| CN107487787B (en) | A kind of hollow KMnF3The preparation method of nanometer square particle |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |