CN102674484A - Preparation method of flower-like alpha-nickel hydroxide - Google Patents
Preparation method of flower-like alpha-nickel hydroxide Download PDFInfo
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- CN102674484A CN102674484A CN2012101698628A CN201210169862A CN102674484A CN 102674484 A CN102674484 A CN 102674484A CN 2012101698628 A CN2012101698628 A CN 2012101698628A CN 201210169862 A CN201210169862 A CN 201210169862A CN 102674484 A CN102674484 A CN 102674484A
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- flower
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- urotropine
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000002815 nickel Chemical class 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- XATZQMXOIQGKKV-UHFFFAOYSA-N nickel;hydrochloride Chemical group Cl.[Ni] XATZQMXOIQGKKV-UHFFFAOYSA-N 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000012716 precipitator Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 9
- 230000036571 hydration Effects 0.000 description 6
- 238000006703 hydration reaction Methods 0.000 description 6
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229910006279 γ-NiOOH Inorganic materials 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- AIYYMMQIMJOTBM-UHFFFAOYSA-L nickel(ii) acetate Chemical class [Ni+2].CC([O-])=O.CC([O-])=O AIYYMMQIMJOTBM-UHFFFAOYSA-L 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
Preparation of flower-shaped alpha-Ni (OH)2Adding nickel salt and urotropine into deionized water, stirring and dissolving, wherein the mass ratio of nickel to urotropine is 1: 1-1: 2, the concentration of nickel salt in the solution is 0.1-1 mol/L, taking 5mL of mixed solution, and then adding 10-35 mL of lower alcohol into the mixed solution; adding deionized water into the obtained solution to a volume of 40mL, transferring the solution into a 50mL high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 2h at 160 ℃, cooling, filtering, washing with deionized hydrated absolute ethyl alcohol for several times respectively, filtering to obtain a product, and drying in a vacuum drying oven at 60 ℃ to obtain flower-shaped alpha-Ni 2. The invention finally prepares pure flower-shaped alpha-Ni (OH) by using urotropine as a precipitator and ethanol as a solvent2。
Description
Technical field
The present invention relates to a kind of preparation method of mineral compound, specifically, is the method that solvent-thermal method prepares flower-shaped class alpha-phase nickel hydroxide.
Background technology
In recent years, discover α-Ni (OH)
2In some aspects than β-Ni (OH)
2Has more advantage, like α-Ni (OH)
2The right charge and discharge cycles of/γ-NiOOH electricity can generating electrodes not expand, and does not have intermediate phase to generate good reversibility in the electric order reaction; α-Ni (OH)
2/ γ-NiOOH electricity is 1.67 to theoretical electron transfer number in the reaction, and its Theoretical Mass specific storage is than β-Ni (OH)
2High.From chemical reaction, the generation of nickel hydroxide is very simple, and under alkali condition, nickel ion combines with hydroxide ion and generates nickel hydroxide precipitate.Yet the nickel hydroxide that generates like this is all to be difficult to reach the requirement of Edison battery to positive electrode material at electrochemical activity or on appearance structure.Therefore, in order to satisfy the requirement of high-capacity battery, prepare high reactivity, highdensity nickel hydroxide anode material becomes present research object.At present, the flower-shape Ni that the document of being reported is prepared (OH)
2Be to be α and β mixed phase mostly, and seldom about preparing pure mutually flower-shaped α-Ni (OH)
2Report.
Summary of the invention
The purpose of this invention is to provide a kind of economical and practical, efficient and environmental protection and prepare flower-shaped α-Ni (OH)
2Method.The present invention is under the environment of lower alcohol, and through adding the precipitation agent urotropine, controlling reaction time and temperature make the nickel salt reaction generate pure mutually flower-shaped α-Ni (OH)
2Technical scheme of the present invention is following:
A kind of method for preparing flower-shaped alpha-nickel hydroxide, it comprises the steps:
Step 1: nickel salt and urotropine are added deionized water for stirring, dissolving, nickel is 1:1 ~ 1:3 with the ratio of the amount of substance of urotropine, the concentration of nickel salt is 0.1 ~ 1 mol/L in the solution;
Step 2: get mixed solution 5 mL in the step 1, add the lower alcohol of 10 ~ 35 mL again;
Step 3: adding deionized water to volume in the solution that step 2 is obtained is 40 mL, is transferred in the autoclave of inner liner polytetrafluoroethylene of 50 mL, and at 160 ℃ down behind reaction 2 h, cooling;
Step 4: the reaction mixture that step 3 is obtained filters, and filters out product for several times with deionized water and absolute ethanol washing respectively again, and places 60 ℃ vacuum drying oven dry, makes flower-shaped α-Ni (OH)
2
Flower-shaped α-the Ni of above-mentioned preparation (OH)
2Method, in the step 1, described nickel salt is 1:2 with the ratio of the preferred amount of substance of urotropine, the concentration of nickel salt is preferably 0.2 ~ 1 mol/L in the solution.
Flower-shaped α-the Ni of above-mentioned preparation (OH)
2Method, in the step 2, described lower alcohol is methyl alcohol, ethanol or propyl alcohol; Add alcohol amount be preferably 25 mL.
Flower-shaped α-the Ni of above-mentioned preparation (OH)
2Method, described nickel salt can be hydrochloric acid nickel, single nickel salt, nickelous nitrate or nickel acetate.
The present invention is precipitation agent with the urotropine, and ethanol is solvent, finally prepares purer flower-shaped α-Ni (OH)
2
Description of drawings
Fig. 1 is the α-Ni (OH) of the inventive method preparation
2The XRD figure picture;
Fig. 2 is the α-Ni (OH) of the inventive method preparation
2The SEM image;
Embodiment:
Embodiment 1
The Nickel dichloride hexahydrate of 0.238 g and the urotropine of 0.280 g are added 5 mL deionized water for stirring, dissolving, the ethanol of adding 25 mL in mixed solution then; With adding deionized water to volume in the solution that obtains is 40 mL; Be transferred in the autoclave of inner liner polytetrafluoroethylene of 50 mL, at 160 ℃ down behind reaction 2 h, cooling; Filter; Spend the ionic hydration absolute ethanol washing more respectively and filter out product for several times, and place 60 ℃ vacuum drying oven dry, make flower-shaped α-Ni (OH)
2Its XRD figure looks like to see Fig. 1, and the SEM image is seen Fig. 2.
Embodiment 2
The Nickelous nitrate hexahydrate of 1.45 g and the urotropine of 0.70 g are added 5 mL deionized water for stirring, dissolving, the methyl alcohol of adding 10 mL in mixed solution then; With adding deionized water to volume in the solution that obtains is 40 mL; Be transferred in the autoclave of inner liner polytetrafluoroethylene of 50 mL, at 160 ℃ down behind reaction 2 h, cooling; Filter; Spend the ionic hydration absolute ethanol washing more respectively and filter out product for several times, and place 60 ℃ vacuum drying oven dry, make flower-shaped α-Ni (OH)
2Its XRD figure picture and SEM image such as embodiment 1.
Embodiment 3
The six hydration nickel sulfate of 0.131 g and the urotropine of 0.210 g are added 5 mL deionized water for stirring, dissolving, the ethanol of adding 35 mL in mixed solution then; With adding deionized water to volume in the solution that obtains is 40 mL; Be transferred in the autoclave of inner liner polytetrafluoroethylene of 50 mL, at 160 ℃ down behind reaction 2 h, cooling; Filter; Spend the ionic hydration absolute ethanol washing more respectively and filter out product for several times, and place 60 ℃ vacuum drying oven dry, make flower-shaped α-Ni (OH)
2Its XRD figure picture and SEM image such as embodiment 1.
Embodiment 4
The four hydration nickel acetates of 0.249 g and the urotropine of 0.280 g are added 5 mL deionized water and stirring, dissolving, the propyl alcohol of adding 20 mL in mixed solution then; With adding deionized water to volume in the solution that obtains is 40 mL; Be transferred in the autoclave of inner liner polytetrafluoroethylene of 50 mL, at 160 ℃ down behind reaction 2 h, cooling; Filter; Spend the ionic hydration absolute ethanol washing more respectively and filter out product for several times, and place 60 ℃ vacuum drying oven dry, make flower-shaped α-Ni (OH)
2Its XRD figure picture and SEM image such as embodiment 1.
Claims (5)
1. the preparation method of a flower-shaped alpha-nickel hydroxide is characterized in that it comprises the steps:
Step 1: nickel salt and urotropine are added deionized water for stirring, dissolving, nickel is 1:1 ~ 1:3 with the ratio of the amount of substance of urotropine, the concentration of nickel salt is 0.1 ~ 1 mol/L in the solution;
Step 2: get mixed solution 5 mL in the step 1, add the lower alcohol of 10 ~ 35 mL again;
Step 3: adding deionized water to volume in the solution that step 2 is obtained is 40 mL, is transferred in the autoclave of inner liner polytetrafluoroethylene of 50 mL, and at 160 ℃ down behind reaction 2 h, cooling;
Step 4: the reaction mixture that step 3 is obtained filters, and filters out product for several times with deionized water and absolute ethanol washing respectively again, and places 60 ℃ vacuum drying oven dry, makes flower-shaped α-Ni (OH)
2
2. the preparation method of flower-shaped alpha-nickel hydroxide according to claim 1, it is characterized in that: in the step 1, described nickel salt is 1:2 with the ratio of the amount of substance of urotropine, and the concentration of nickel salt is 0.2 ~ 1 mol/L in the solution.
3. the preparation method of flower-shaped alpha-nickel hydroxide according to claim 1, it is characterized in that: in the step 2, described lower alcohol is methyl alcohol, ethanol or propyl alcohol.
4. the preparation method of flower-shaped alpha-nickel hydroxide according to claim 1 is characterized in that: the described amount that adds alcohol of step 2 is 25 mL.
5. the preparation method of flower-shaped alpha-nickel hydroxide according to claim 1, it is characterized in that: described nickel salt is hydrochloric acid nickel, single nickel salt, nickelous nitrate or nickel acetate.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104409791A (en) * | 2014-11-14 | 2015-03-11 | 广东华科新材料研究院有限公司 | Method for preparation of flower-like nickel hydroxide electrode material from waste battery |
| CN104610998A (en) * | 2013-12-19 | 2015-05-13 | 北京林业大学 | Method for preparing biodiesel by employing flower-like nickel-based catalyst material |
| CN105251434A (en) * | 2015-11-12 | 2016-01-20 | 安徽师范大学 | Synthesizing method for flower-shaped nickel-based nano material with high-selectivity adsorption and separation on methyl orange |
| CN105384198A (en) * | 2015-12-17 | 2016-03-09 | 宁波繁盛商业管理有限公司 | Method for preparation of alpha-phase nickel hydroxide microsphere |
| CN106745133A (en) * | 2017-01-24 | 2017-05-31 | 武汉工程大学 | A kind of preparation method of water insoluble hydroxide |
| CN107123554A (en) * | 2016-02-25 | 2017-09-01 | 中国科学院苏州纳米技术与纳米仿生研究所 | Flexible electrode, its preparation method and application |
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| CN101723473A (en) * | 2009-11-11 | 2010-06-09 | 北京化工大学 | Preparation method of multivariate doping spherical alpha-Ni(OH)2 with nanometer secondary structure |
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| CN101723473A (en) * | 2009-11-11 | 2010-06-09 | 北京化工大学 | Preparation method of multivariate doping spherical alpha-Ni(OH)2 with nanometer secondary structure |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610998A (en) * | 2013-12-19 | 2015-05-13 | 北京林业大学 | Method for preparing biodiesel by employing flower-like nickel-based catalyst material |
| CN104610998B (en) * | 2013-12-19 | 2017-07-04 | 北京林业大学 | A kind of method that biodiesel is prepared using flower-shaped nickel catalyst agent material |
| CN104409791A (en) * | 2014-11-14 | 2015-03-11 | 广东华科新材料研究院有限公司 | Method for preparation of flower-like nickel hydroxide electrode material from waste battery |
| CN104409791B (en) * | 2014-11-14 | 2016-05-18 | 广东华科新材料研究院有限公司 | Prepare the method for flower-shaped nickel hydroxide electrode material from waste battery |
| CN105251434A (en) * | 2015-11-12 | 2016-01-20 | 安徽师范大学 | Synthesizing method for flower-shaped nickel-based nano material with high-selectivity adsorption and separation on methyl orange |
| CN105251434B (en) * | 2015-11-12 | 2018-01-16 | 安徽师范大学 | The synthetic method of the flower-shaped nickel base nanometer material of methyl orange high-selectivity adsorption separation |
| CN105384198A (en) * | 2015-12-17 | 2016-03-09 | 宁波繁盛商业管理有限公司 | Method for preparation of alpha-phase nickel hydroxide microsphere |
| CN107123554A (en) * | 2016-02-25 | 2017-09-01 | 中国科学院苏州纳米技术与纳米仿生研究所 | Flexible electrode, its preparation method and application |
| CN107123554B (en) * | 2016-02-25 | 2019-12-06 | 中国科学院苏州纳米技术与纳米仿生研究所 | flexible electrode, manufacturing method and application thereof |
| CN106745133A (en) * | 2017-01-24 | 2017-05-31 | 武汉工程大学 | A kind of preparation method of water insoluble hydroxide |
| CN106745133B (en) * | 2017-01-24 | 2018-03-20 | 武汉工程大学 | A kind of preparation method of hydroxide not soluble in water |
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Application publication date: 20120919 |