CN109336190A - A kind of rapid precipitation prepares one-dimensional CoCO3Method - Google Patents

A kind of rapid precipitation prepares one-dimensional CoCO3Method Download PDF

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Publication number
CN109336190A
CN109336190A CN201811532163.9A CN201811532163A CN109336190A CN 109336190 A CN109336190 A CN 109336190A CN 201811532163 A CN201811532163 A CN 201811532163A CN 109336190 A CN109336190 A CN 109336190A
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CN
China
Prior art keywords
coco
dimensional
water
rapid precipitation
naco
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Pending
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CN201811532163.9A
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Chinese (zh)
Inventor
侴术雷
赖伟鸿
王云晓
李用成
李东祥
李亚书
宫毅涛
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Liaoning Xingkong Sodium Battery Co Ltd
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Liaoning Xingkong Sodium Battery Co Ltd
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Priority to CN201811532163.9A priority Critical patent/CN109336190A/en
Publication of CN109336190A publication Critical patent/CN109336190A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/06—Carbonates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Abstract

The present invention relates to technical field of nanometer material preparation, and disclose a kind of rapid precipitation and prepare one-dimensional CoCO3Method, comprising the following steps: S1, by 0.048M Co (NO3)2It is dissolved in 15ml water and stirs evenly, then the temperature was then adjusted to 80 DEG C and keep constant；S2, again by 0.124M NaCO3It in the 15ml water of dissolution in step 1 and stirs evenly, until a large amount of visible purple precipitatings are precipitated in two kinds of solution mixing；S3, with water and ethyl alcohol by purple washing of precipitate for several times, recycle vacuum drying oven with 60 DEG C drying to get high-purity monodimension nanometer material CoCO3.The rapid precipitation prepares one-dimensional CoCO3Method, utilize sodium carbonate (NaCO3) it is that precipitating reagent rapid precipitation goes out target material, prepare that such material is fast with reaction rate, react mild easily-controllable, energy conservation and environmental protection, product purity height and the advantages such as novel in shape using the precipitation method.The process route is not only CoCO3Investigation of materials and application provide scientific research foundation, while also providing reliable guarantee to explore the rule between material microscopic appearance and performance boost.

Description

A kind of rapid precipitation prepares one-dimensional CoCO3Method
Technical field
The present invention relates to technical field of nanometer material preparation, specially a kind of rapid precipitation prepares one-dimensional CoCO3Method.
Background technique
CoCO3Belong to metal carbonate, because its special crystal structure and its Derived Oxides are urging this substance The fields such as change, energy storage have extensive potential application.Rapid, high volume prepares the preparation of this electrode material and ionic conductor material synthesis Field has extensive use.Especially, special one-dimentional structure has the electronic and ionic conduction orientation of orientation, powerful stress Ability to bear and short axial ion transmission path, it is considered to be particularly significant nano material branch.
Summarize through Literature Consult, it is existing to prepare one-dimensional CoCO3The method of nano material is more rare, and CoCO is reported in part3It receives The preparation of rice material is mainly based upon CoCO3Three-dimensional nanoparticles synthesis (C.C.Li, X.M.Yin, T.H.Wang, H.C.Zeng,Chemistry of Materials 2009,21,4984-4992；M.Y.Nassar,Materials Letters 2013,94,112-115；L.Su,Z.Zhou,X.Qin,Q.Tang,D.Wu,P.Shen,Nano Energy 2013,2,276-282；Z.Ding,B.Yao,J.Feng,J.Zhang,Journal of Materials Chemistry A 2013,1,11200-11209)。
Therefore, one-dimensional CoCO can simply, quickly be prepared by inventing one kind3The method of nano material will be in following industry Change, and widely applies production particularly important.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of rapid precipitations to prepare one-dimensional CoCO3Method, have benefit With sodium carbonate (NaCO3) it is precipitating reagent rapid precipitation the advantages that going out target material, it solves and existing prepares one-dimensional CoCO3Nanometer material The method of material is more rare, and CoCO is reported in part3The preparation of nano material is mainly based upon CoCO3Three-dimensional nanoparticles synthesis Problem.
(2) technical solution
Sodium carbonate (NaCO is utilized for realization is above-mentioned3) it is the purpose of precipitating reagent rapid precipitation goes out target material, the present invention mentions For following technical solution: a kind of rapid precipitation prepares one-dimensional CoCO3Method, this method is with Co (NO3)2And NaCO3For raw material, Distilled water is solvent, is synthesized using liquid-phase precipitation method, comprising the following steps:
S1, by 0.048M Co (NO3)2It is dissolved in 15ml water and stirs evenly, then the temperature was then adjusted to 80 DEG C and keep It is constant；
S2, again by 0.124M NaCO3It in the 15ml water of dissolution in step 1 and stirs evenly, until two kinds of solution mixing A large amount of visible purple precipitatings are precipitated；
S3, with water and ethyl alcohol by purple washing of precipitate for several times, recycle vacuum drying oven with 60 DEG C drying to get high-purity one Dimension nano material CoCO3。
This method has a variety of outstanding features such as efficient, quick, succinct in preparing material, overcomes the fast of precipitation reaction The huge challenge of regulation monodimension nanometer material, prepares monodimension nanometer material CoCO caused by fast crystallization3, utilize sodium carbonate (NaCO3) it is that precipitating reagent rapid precipitation goes out target material.
(3) beneficial effect
Compared with prior art, the present invention provides a kind of rapid precipitations to prepare one-dimensional CoCO3Method, having following has Beneficial effect:
1, the rapid precipitation prepares one-dimensional CoCO3Method, utilize sodium carbonate (NaCO3) it is that precipitating reagent rapid precipitation goes out mesh Material is marked, it is high to prepare such material fast with reaction rate, the mild easily-controllable, energy conservation and environmental protection of reaction, product purity using the precipitation method And the advantages such as novel in shape.The process route is not only CoCO3Investigation of materials and application provide scientific research foundation, while being also exploration Rule between material microscopic appearance and performance boost provides reliable guarantee.
2, the rapid precipitation prepares one-dimensional CoCO3Method, use liquid phase low-temperature precipitation method carry out material preparation, this method It is at low cost, fast, easy to operate, the mild easily-controllable, energy conservation and environmental protection of reaction rate, product purity height and novel in shape；And it is prepared Product be 1-dimention nano needle construction, nanoneedle draw ratio is big, quality is stable, with high purity, manufacturing cost is low, specific surface area is significant Increase.
Detailed description of the invention
Fig. 1 is CoCO in embodiment3Nanoneedle X-ray diffraction (XRD) figure；
Fig. 2 is CoCO in embodiment3Nanoneedle scanning electron microscope (SEM) test chart；
Fig. 3 is CoCO in embodiment3Nanoneedle projection electron microscope (TEM) test chart.
Specific embodiment
Below in conjunction with the embodiment of the present invention and attached drawing, technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
Embodiment: a kind of rapid precipitation prepares one-dimensional CoCO3Method, this method is with Co (NO3)2And NaCO3For raw material, Distilled water is solvent, is synthesized using liquid-phase precipitation method, comprising the following steps:
S1, by 0.048M Co (NO3)2It is dissolved in 15ml water and stirs evenly, then the temperature was then adjusted to 80 DEG C and keep It is constant；
S2, again by 0.124M NaCO3It in the 15ml water of dissolution in step 1 and stirs evenly, until two kinds of solution mixing A large amount of visible purple precipitatings are precipitated；
S3, with water and ethyl alcohol by purple washing of precipitate for several times, recycle vacuum drying oven with 60 DEG C drying to get high-purity one Dimension nano material CoCO3(see attached drawing 1-3).
This method has a variety of outstanding features such as efficient, quick, succinct in preparing material, overcomes the fast of precipitation reaction The huge challenge of regulation monodimension nanometer material, prepares monodimension nanometer material CoCO caused by fast crystallization3, utilize sodium carbonate (NaCO3) it is that precipitating reagent rapid precipitation goes out target material.
The rapid precipitation prepares one-dimensional CoCO3Method, utilize sodium carbonate (NaCO3) it is that precipitating reagent rapid precipitation goes out target Material, prepare that such material is fast with reaction rate, it is high to react mild easily-controllable, energy conservation and environmental protection, product purity using the precipitation method and The advantages such as novel in shape.The process route is not only CoCO3Investigation of materials and application provide scientific research foundation, while being also exploration material Rule between material microscopic appearance and performance boost provides reliable guarantee, solves and existing prepares one-dimensional CoCO3Nano material Method is more rare, and CoCO is reported in part3The preparation of nano material is mainly based upon CoCO3The problem of three-dimensional nanoparticles synthesize.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (1)

1. a kind of rapid precipitation prepares one-dimensional CoCO3Method, which comprises the following steps:
S1, by 0.048M Co (NO3)2It is dissolved in 15ml water and stirs evenly, then the temperature was then adjusted to 80 DEG C and keep constant；
S2, again by 0.124M NaCO3It in the 15ml water of dissolution in step 1 and stirs evenly, until two kinds of solution mixing are precipitated A large amount of visible purple precipitatings；
S3, with water and ethyl alcohol by purple washing of precipitate for several times, recycle vacuum drying oven with 60 DEG C drying to get one wiener of high-purity Rice material C oCO3。
CN201811532163.9A 2018-12-14 2018-12-14 A kind of rapid precipitation prepares one-dimensional CoCO3Method Pending CN109336190A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110540251A (en) * 2019-09-06 2019-12-06 辽宁星空钠电电池有限公司 method for preparing one-dimensional cobalt carbonate by rapid precipitation

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006116251A2 (en) * 2005-04-26 2006-11-02 The University Of Chicago Processes for making dense, spherical, active materials for lithium-ion cells
CN101343084B (en) * 2008-08-20 2010-06-02 周红阳 Process for preparing high-density cobaltous carbonate
CN202007231U (en) * 2011-01-29 2011-10-12 黄桂忠 Quick precipitator
CN106927488A (en) * 2017-05-03 2017-07-07 中南大学 A kind of preparation method of cobalt carbonate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006116251A2 (en) * 2005-04-26 2006-11-02 The University Of Chicago Processes for making dense, spherical, active materials for lithium-ion cells
CN101343084B (en) * 2008-08-20 2010-06-02 周红阳 Process for preparing high-density cobaltous carbonate
CN202007231U (en) * 2011-01-29 2011-10-12 黄桂忠 Quick precipitator
CN106927488A (en) * 2017-05-03 2017-07-07 中南大学 A kind of preparation method of cobalt carbonate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110540251A (en) * 2019-09-06 2019-12-06 辽宁星空钠电电池有限公司 method for preparing one-dimensional cobalt carbonate by rapid precipitation

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