CN103466725B - 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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- CN103466725B CN103466725B CN201310402021.1A CN201310402021A CN103466725B CN 103466725 B CN103466725 B CN 103466725B CN 201310402021 A CN201310402021 A CN 201310402021A CN 103466725 B CN103466725 B CN 103466725B
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- Prior art keywords
- flower
- microsphere
- nickel chloride
- basic nickel
- nickelous chloride
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- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 title claims abstract description 38
- 239000004005 microsphere Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 13
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 title abstract 6
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims abstract description 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 239000003513 alkali Substances 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 2
- 229960004217 benzyl alcohol Drugs 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 7
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000002135 nanosheet Substances 0.000 abstract 2
- 238000005119 centrifugation Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 11
- 239000000843 powder Substances 0.000 description 10
- 206010013786 Dry skin Diseases 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910052599 brucite Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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 preparing alkali formula nickelous chloride flower-like microsphere.
Background technology
The nanostructure of morphology controllable is in catalysis, and gas sensor, lithium ion battery, the fields such as photoelectric device are widely used.3 D complex micro-nano structure can combine the performance of the performance of material micron yardstick and nanoscale, thus gives material new performance.As a kind of special 3 D complex structure, three-dimensional flower-shaped structure because it is at ultracapacitor, water treatment, the application in lithium ion battery and especially noticeable.Although 3 D complex structure has lot of advantages, their controlledly synthesis remains the ultimate challenge faced by researchist.
Stratified material has a lot of effective active ducts and very large specific surface area, and due to the crystalline structure that they are special, they are easy to form sheet structure or flower-like structure.Alkali formula nickelous chloride is a kind of stratified material, have class brucite structure, but its crystalline structure is not determined.In order to study crystalline structure and its growth behavior of this novel material, be necessary that exploitation is simple, repeatably synthetic method.In the past, researchist adopts the alkaline matter of nickelous chloride and certain proportioning, by replacement(metathesis)reaction synthetic alkali formula nickelous chloride.But what this reaction was formed is usually the mixture of various non-stoichiometric alkali formula nickelous chloride.Therefore, synthesis purity is high, and the alkali formula nickelous chloride structure that pattern integrity is good is significant.
Summary of the invention
The object of this invention is to provide a kind of method simply preparing alkali formula nickelous chloride flower-like microsphere without the need to template, technique.
The method preparing alkali formula nickelous chloride flower-like microsphere of the present invention, comprises the following steps:
1) be dissolved in organic solvent by Nickel dichloride hexahydrate, Nickel dichloride hexahydrate volumetric molar concentration is in organic solvent 0.01 ~ 1 M, is stirred to and evenly obtains settled solution;
2) solution that step 1) is obtained is transferred in solvent thermal device, at 100 ~ 200 DEG C, carry out solvent thermal reaction 5 min ~ 100 h, centrifugal, dry, obtain alkali formula nickelous chloride flower-like microsphere.
Above-mentioned organic solvent can be ethanol, or the mixed solution of one or more in ethanol and methyl alcohol, ethanol, propyl alcohol, butanols, normal hexane, hexanaphthene, phenylcarbinol, toluene, acetone and tetrahydrofuran (THF).
The alkali formula nickelous chloride flower-like microsphere that the inventive method obtains is made up of alkali formula nickelous chloride nanometer sheet, and these nanometer sheet are made up of nano particle, comprise a large amount of pore passage structures in nanometer sheet.Building-up process of the present invention is without the need to masterplate, and without the need to subsequent disposal, required equipment is simple, and cost is low, and productive rate is high, easily extensive synthesis.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the alkali formula nickelous chloride flower-like microsphere of embodiment 1.
Fig. 2 is the X-ray energy dispersion spectrum of the alkali formula nickelous chloride flower-like microsphere of embodiment 1.
Fig. 3 is the stereoscan photograph of the alkali formula nickelous chloride flower-like microsphere of embodiment 1.
Fig. 4 is the transmission electron microscope photo of the alkali formula nickelous chloride flower-like microsphere 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 that step 1) is obtained is transferred in solvent thermal device, at 170 DEG C, carry out the solvent thermal reaction of 6 h, then gained material is carried out centrifugal, then 80 DEG C of dryings, obtain 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 substance 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 this illustrates that the chemical formula of 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 that step 1) is obtained is transferred in solvent thermal device, at 180 DEG C, carry out the solvent thermal reaction of 9 h, then gained material is carried out centrifugal, then 80 DEG C of dryings, obtain alkali formula nickelous chloride powder.
Prepare the transmission electron microscope photo of alkali formula nickelous chloride as shown in Fig. 4.As can be seen from photo, alkali formula nickelous chloride flower-like microsphere is made up of alkali formula nickelous chloride nanometer sheet, and these nanometer sheet are made up 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 that step 1) is obtained is transferred in solvent thermal device, at 130 DEG C, carry out the solvent thermal reaction of 100 h, then gained material is carried out centrifugal, then 80 DEG C of dryings, obtain alkali formula nickelous chloride powder.
Embodiment 4
1) 1.08 g Nickel dichloride hexahydrates are dissolved in 30 ml ethanol, are stirred to and evenly obtain settled solution.
2) solution that step 1) is obtained is transferred in solvent thermal device, at 200 DEG C, carry out the solvent thermal reaction of 10 min, then gained material is carried out centrifugal, then 80 DEG C of dryings, obtain 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 that step 1) is obtained is transferred in solvent thermal device, at 170 DEG C, carry out the solvent thermal reaction of 12 h, then gained material is carried out centrifugal, then 80 DEG C of dryings, obtain 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 that step 1) is obtained is transferred in solvent thermal device, at 170 DEG C, carry out the solvent thermal reaction of 6 h, then gained material is carried out centrifugal, then 80 DEG C of dryings, obtain alkali formula nickelous chloride powder.
Claims (1)
1. prepare a method for alkali formula nickelous chloride flower-like microsphere, it is characterized in that comprising the following steps:
1) be dissolved in organic solvent by Nickel dichloride hexahydrate, Nickel dichloride hexahydrate volumetric molar concentration is in organic solvent 0.01 ~ 1 M, is stirred to and evenly obtains settled solution; Described organic solvent is ethanol, or the mixed solution of one or more in ethanol and methyl alcohol, propyl alcohol, butanols, normal hexane, hexanaphthene, phenylcarbinol, toluene, acetone and tetrahydrofuran (THF);
2) solution that step 1) is obtained is transferred in solvent thermal device, at 100 ~ 200 DEG C, carry out solvent thermal reaction 5 min ~ 100 h, centrifugal, dry, obtain alkali formula nickelous chloride flower-like microsphere.
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| Application Number | Priority Date | Filing Date | Title |
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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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| CN201310402021.1A CN103466725B (en) | 2013-09-06 | 2013-09-06 | Method of preparing basic nickel chloride flower-like microsphere |
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| CN103466725A CN103466725A (en) | 2013-12-25 |
| CN103466725B true CN103466725B (en) | 2015-07-15 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109537053B (en) * | 2018-11-21 | 2020-04-17 | 湖南大学 | Ultrathin single crystal NiCl2Nanosheet and preparation method and application thereof |
| CN113526575B (en) * | 2021-09-07 | 2022-05-31 | 吉林大学 | Nickel hydroxychloride nano material and preparation method thereof |
| CN114988498B (en) * | 2022-07-06 | 2023-05-16 | 吉林大学 | Nickel hydroxychloride micron flower 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 |
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| CN103466725A (en) | 2013-12-25 |
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Granted publication date: 20150715 Termination date: 20210906 |