CN103466725A - Method of preparing basic nickel chloride flower-like microsphere - Google Patents
Method of preparing basic nickel chloride flower-like microsphere Download PDFInfo
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- CN103466725A CN103466725A CN2013104020211A CN201310402021A CN103466725A CN 103466725 A CN103466725 A CN 103466725A CN 2013104020211 A CN2013104020211 A CN 2013104020211A CN 201310402021 A CN201310402021 A CN 201310402021A CN 103466725 A CN103466725 A CN 103466725A
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Abstract
The invention discloses a method of preparing a basic nickel chloride flower-like microsphere. The method comprises the steps of dissolving nickel chloride hexahydrate in an organic solvent firstly, transferring the solution into a solvent heating device to carry out solvent-thermal reaction, and then, carrying out centrifugation and drying on a substance obtained after the solvent-thermal reaction to obtain the basic nickel chloride flower-like microsphere. The prepared basic nickel chloride flower-like microsphere consists of basic nickel chloride nano-sheets, each nano-sheet consists of nano-particles and comprises a great deal of channel structures. According to the method disclosed by the invention, a template and subsequent treatment are not needed in the synthetic process, the needed equipment is simple, the cost is low, the yield is high, and the basic nickel chloride flower-like microspheres are easily synthesized in a large scale.
Description
Technical field
The present invention relates to a kind of method for preparing the flower-shaped microballoon of alkali formula nickelous chloride.
Background technology
The controlled nanostructure of pattern is in catalysis, gas sensor, and lithium ion battery, the fields such as photoelectric device are widely used.The 3 D complex micro-nano structure can combine the performance of the performance of material micron yardstick and nanoscale, thereby gives the performance that material is new.As a kind of special 3 D complex structure, three-dimensional flower-shaped structure because its at ultracapacitor, water treatment, the application in lithium ion battery and especially noticeable.Although the 3 D complex structure has lot of advantages, their controlledly synthesis remains the ultimate challenge that the researchist faces.
Stratified material has a lot of effective active ducts and very large specific surface area, and due to they special crystalline structure, they are easy to form sheet structure or flower-like structure.Alkali formula nickelous chloride is a kind of stratified material, has class brucite structure, but its crystalline structure is not determined.For the crystalline structure of studying this novel material and its growth behavior, be necessary that exploitation is simple, repeatably synthetic method.In the past, the researchist adopts the alkaline matter of nickelous chloride and certain proportioning, by replacement(metathesis)reaction synthetic alkali formula nickelous chloride.Yet what this reaction formed is usually the mixture of various non-stoichiometric alkali formula nickelous chlorides.Therefore, synthetic purity is high, and the alkali formula nickelous chloride structure that complete shape and appearance is good is significant.
Summary of the invention
The purpose of this invention is to provide a kind of method that simply prepares the flower-shaped microballoon of alkali formula nickelous chloride without template, technique.
The method for preparing the flower-shaped microballoon of alkali formula nickelous chloride of the present invention comprises the following steps:
1) Nickel dichloride hexahydrate is dissolved in organic solvent, the volumetric molar concentration of Nickel dichloride hexahydrate in organic solvent is 0.01 ~ 1 M, is stirred to and evenly obtains settled solution;
2) solution step 1) made is transferred in the solvent thermal device, carries out solvent thermal reaction 5 min～100 h under 100 ~ 200 ℃, centrifugal, and drying obtains the flower-shaped microballoon of alkali formula nickelous chloride.
Above-mentioned organic solvent can be ethanol, or one or more the mixed solution in ethanol and methyl alcohol, ethanol, propyl alcohol, butanols, normal hexane, hexanaphthene, phenylcarbinol, toluene, acetone and tetrahydrofuran (THF).
The flower-shaped microballoon of alkali formula nickelous chloride that the inventive method makes is comprised of alkali formula nickelous chloride nanometer sheet, and these nanometer sheet are comprised of nano particle, comprise a large amount of pore passage structures in nanometer sheet.Building-up process of the present invention is without masterplate, and without subsequent disposal, required equipment is simple, and cost is low, and productive rate is high, easily extensive synthetic.
The accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the flower-shaped microballoon of alkali formula nickelous chloride of embodiment 1.
Fig. 2 is the X ray energy dispersion spectrum of the flower-shaped microballoon of alkali formula nickelous chloride of embodiment 1.
Fig. 3 is the stereoscan photograph of the flower-shaped microballoon of alkali formula nickelous chloride of embodiment 1.
Fig. 4 is the transmission electron microscope photo of the flower-shaped microballoon of alkali formula nickelous chloride of embodiment 2.
Embodiment
Embodiment 1
1) 1.08 g Nickel dichloride hexahydrates are dissolved in 30 ml ethanol, are stirred to and evenly obtain settled solution.
2) solution step 1) made is transferred in the solvent thermal device, carries out the solvent thermal reaction of 6 h under 170 ℃, then the gained material is carried out centrifugal, then 80 ℃ of dryings, obtains alkali formula nickelous chloride powder.
The X ray diffracting spectrum of the alkali formula nickelous chloride powder of preparation is as shown in Fig. 1.This collection of illustrative plates can not mate with the standard diagram of any known phase.The X ray energy dispersion spectrum of the alkali formula nickelous chloride powder of preparation as shown in Figure 2.Known by X ray energy dispersion spectrum, the mol ratio of Ni:Cl:O is about 1:1:1, and the chemical formula of this explanation alkali formula nickelous chloride is NiCl (OH).The stereoscan photograph of the alkali formula nickelous chloride powder of preparation as shown in Figure 3.As can be seen from the figure, the alkali formula nickelous chloride powder of preparation has good flower-like structure.
Embodiment 2
1) 1.08 g Nickel dichloride hexahydrates are dissolved in 30 ml ethanol, are stirred to and evenly obtain settled solution.
2) solution step 1) made is transferred in the solvent thermal device, carries out the solvent thermal reaction of 9 h under 180 ℃, then the gained material is carried out centrifugal, then 80 ℃ of dryings, obtains alkali formula nickelous chloride powder.
Prepare the transmission electron microscope photo of alkali formula nickelous chloride as shown in Fig. 4.From photo, can find out, the flower-shaped microballoon of alkali formula nickelous chloride is comprised of alkali formula nickelous chloride nanometer sheet, and these nanometer sheet are comprised of nano particle, comprise a large amount of pore passage structures in nanometer sheet.
Embodiment 3
1) 1.08 g Nickel dichloride hexahydrates are dissolved in 30 ml ethanol, are stirred to and evenly obtain settled solution.
2) solution step 1) made is transferred in the solvent thermal device, carries out the solvent thermal reaction of 100 h under 130 ℃, then the gained material is carried out centrifugal, then 80 ℃ of dryings, obtains alkali formula nickelous chloride powder.
1) 1.08 g Nickel dichloride hexahydrates are dissolved in 30 ml ethanol, are stirred to and evenly obtain settled solution.
2) solution step 1) made is transferred in the solvent thermal device, carries out the solvent thermal reaction of 10 min under 200 ℃, then the gained material is carried out centrifugal, then 80 ℃ of dryings, obtains alkali formula nickelous chloride powder.
Embodiment 5
1) 0.54 g Nickel dichloride hexahydrate is dissolved in 30 ml ethanol, is stirred to and evenly obtains settled solution.
2) solution step 1) made is transferred in the solvent thermal device, carries out the solvent thermal reaction of 12 h under 170 ℃, then the gained material is carried out centrifugal, then 80 ℃ of dryings, obtains alkali formula nickelous chloride powder.
Embodiment 6
1) 1.08 g Nickel dichloride hexahydrates are dissolved in the mixing solutions of 15 ml methyl alcohol and 15ml ethanol, are stirred to and evenly obtain settled solution.
2) solution step 1) made is transferred in the solvent thermal device, carries out the solvent thermal reaction of 6 h under 170 ℃, then the gained material is carried out centrifugal, then 80 ℃ of dryings, obtains alkali formula nickelous chloride powder.
Claims (2)
1. a method for preparing the flower-shaped microballoon of alkali formula nickelous chloride is characterized in that comprising the following steps:
1) Nickel dichloride hexahydrate is dissolved in organic solvent, the volumetric molar concentration of Nickel dichloride hexahydrate in organic solvent is 0.01 ~ 1 M, is stirred to and evenly obtains settled solution;
2) solution step 1) made is transferred in the solvent thermal device, carries out solvent thermal reaction 5 min～100 h under 100 ~ 200 ℃, centrifugal, and drying obtains the flower-shaped microballoon of alkali formula nickelous chloride.
2. according to the described method for preparing the flower-shaped microballoon of alkali formula nickelous chloride of claim 1, it is characterized in that described organic solvent is ethanol, or one or more the mixed solution in ethanol and methyl alcohol, propyl alcohol, butanols, normal hexane, hexanaphthene, phenylcarbinol, toluene, acetone and tetrahydrofuran (THF).
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| CN201310402021.1A CN103466725B (en) | 2013-09-06 | 2013-09-06 | Method of preparing basic nickel chloride flower-like microsphere |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109537053A (en) * | 2018-11-21 | 2019-03-29 | 湖南大学 | A kind of ultra thin single crystalline NiCl2Nanometer sheet and its preparation method and application |
| CN113526575A (en) * | 2021-09-07 | 2021-10-22 | 吉林大学 | Nickel hydroxychloride nano material and preparation method thereof |
| CN114988498A (en) * | 2022-07-06 | 2022-09-02 | 吉林大学 | Nickel hydroxychloride micro-flowers and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417823A (en) * | 2008-11-14 | 2009-04-29 | 中国科学院上海硅酸盐研究所 | Wet chemical preparation method of nickel oxide hollow microsphere without template |
| CN101985367A (en) * | 2010-07-28 | 2011-03-16 | 中国科学院上海硅酸盐研究所 | Method for preparing multilayer alpha-Ni(OH)2 or NiO nanocrystal by microwave solvothermal method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417823A (en) * | 2008-11-14 | 2009-04-29 | 中国科学院上海硅酸盐研究所 | Wet chemical preparation method of nickel oxide hollow microsphere without template |
| CN101985367A (en) * | 2010-07-28 | 2011-03-16 | 中国科学院上海硅酸盐研究所 | Method for preparing multilayer alpha-Ni(OH)2 or NiO nanocrystal by microwave solvothermal method |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109537053A (en) * | 2018-11-21 | 2019-03-29 | 湖南大学 | A kind of ultra thin single crystalline NiCl2Nanometer sheet and its preparation method and application |
| CN109537053B (en) * | 2018-11-21 | 2020-04-17 | 湖南大学 | Ultrathin single crystal NiCl2Nanosheet and preparation method and application thereof |
| CN113526575A (en) * | 2021-09-07 | 2021-10-22 | 吉林大学 | Nickel hydroxychloride nano material and preparation method thereof |
| CN114988498A (en) * | 2022-07-06 | 2022-09-02 | 吉林大学 | Nickel hydroxychloride micro-flowers and preparation method thereof |
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| CN103466725B (en) | 2015-07-15 |
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