CN101624215B - Method for preparing nano nickel oxide - Google Patents
Method for preparing nano nickel oxide Download PDFInfo
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- CN101624215B CN101624215B CN2008101164446A CN200810116444A CN101624215B CN 101624215 B CN101624215 B CN 101624215B CN 2008101164446 A CN2008101164446 A CN 2008101164446A CN 200810116444 A CN200810116444 A CN 200810116444A CN 101624215 B CN101624215 B CN 101624215B
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Abstract
The invention relates to a method for preparing nano nickel oxide. The method adopts inorganic salt to prevent sintering growth of nickel oxide crystals and grains. The prepared nano nickel oxide has small grain size and better heat-resistant property; a surfactant is not used in a preparation process of the nano nickel oxide; and the used inorganic salt is easy to reclaim.
Description
Technical field
The present invention relates to the preparation method of nano-nickel oxide.
Background technology
Nano-nickel oxide has big specific surface area and pore volume and is in crystal boundary in a large number and the central atom of intragranular defective, is the important inorganic materials that is widely used in fields such as battery electrode, catalyzer, magneticsubstance and ceramic coloring material.The particle of nano-nickel oxide is little, specific surface area is big, anti-caking power a little less than.
At present, through using tensio-active agent to realize, the preparation process is complicated mostly in the preparation of nano-nickel oxide.Chinese invention patent " solid phase interface induced precipitation prepares the method for nickel oxide, cobalt oxide powder " (application number 200510031532.2) discloses a kind of method for preparing nickel oxide powder.At first prepare certain density soluble nickel salt brine solution; Add a certain amount of macromolecule dispersing agent such as OP, PVP etc.; Property or add the oxalate powder of certain granules degree several times again after mixing; Regulate pH value between 1.0～5.0, reaction, ageing at a certain temperature, calcining obtains nickel oxide powder again.The granularity of utilizing the nickel oxide powder that this method obtains is about several microns.Chinese invention patent " is used for nickel oxide of electrochemical capacitor and preparation method thereof ", and (application number 200610019323.0) announced a kind of method for preparing high-ratio surface, high specific volume nickel oxide.Adopting nickelous nitrate is the nickel source, and sodium oxalate and sodium hydroxide are precipitation agent, and tween-80 is a tensio-active agent, through liquid-phase precipitation, wear out and 250～350 ℃ of processes such as thermolysis to make grain size be 8～15nm nickel oxide nano particle, specific surface area is 150～250m
2/ g.This method can prepare nano oxidized nickel material, but in the preparation process, need to use tensio-active agent, and has that the preparation process is complicated, tensio-active agent is difficult to reclaim, environment is unfriendly and shortcoming such as resistance to elevated temperatures is relatively poor.
Summary of the invention
The invention provides the preparation method of two kinds of nano-nickel oxides, these two kinds of methods all adopt the difficult inorganic salt that decompose to prevent that the sintering of nickel oxide crystal grain from growing up, and in the preparation process of nano-nickel oxide, need not use tensio-active agent.
The preparation method of first kind of nano-nickel oxide provided by the invention may further comprise the steps:
(1) with the precipitation agent aqueous solution and nickel salt aqueous solution reaction, generates deposition;
(2) inorganic salt with water soluble and heat decomposition temperature＞300 ℃ add in the system of steps (1), and evaporate to dryness water obtains mixture;
(3) with the mixture porphyrize of step (2), after drying, the roasting, washing obtains nano-nickel oxide through drying again;
Said precipitation agent is in water, to produce OH
-, CO
3 2-Or
-OOCCOO
-Material.
Precipitation agent is selected from one or more in ammoniacal liquor, urea, sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood, volatile salt, bicarbonate of ammonia, oxalic acid, sodium oxalate and the potassium oxalate.
The concentration of precipitation agent is 0.05～3mol/L, is preferably 0.5～2mol/L.
Nickel salt in the step (1) is selected from water soluble nickel salt, for example one or more in nickelous nitrate, nickelous chloride, nickelous bromide, nickelous iodide and the single nickel salt.
The concentration of nickel salt aqueous solution is 0.05～3mol/L, is preferably 0.5～2mol/L.
The mol ratio of precipitation agent and nickel salt is 1: 1～3: 1.
Inorganic salt in the step (2) are preferably one or more in sodium-chlor, Repone K, sodium sulfate, vitriolate of tartar, sodium phosphate and the potassiumphosphate.
In the step (2), the mol ratio of inorganic salt and nickel salt is 0.1～2: 1, is preferably 0.2～1.2: 1.
In the step (3), drying temperature is 80～130 ℃, and be 6～8h time of drying; Maturing temperature is 300～600 ℃, and roasting time is 2～8h.
The preparation method of second kind of nano nickel oxide particles provided by the invention may further comprise the steps:
(1) with the precipitation agent aqueous solution and nickel salt aqueous solution reaction, generates deposition, after filtration, washing, drying, obtain the nickel oxide precursor powder;
(2) inorganic salt with the nickel oxide precursor powder of gained in the step (1) and water soluble and heat decomposition temperature＞300 ℃ mix, grinding, and roasting is washed, and obtains nano nickel oxide particles after the drying;
Said precipitation agent is in water, to produce OH
-, CO
3 2-Or
-OOCCOO
-Material.
Precipitation agent is selected from one or more in ammoniacal liquor, urea, sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood, volatile salt, bicarbonate of ammonia, oxalic acid, sodium oxalate and the potassium oxalate.
The concentration of precipitation agent is 0.05～3mol/L, is preferably 0.5～2mol/L.
Nickel salt in the step (1) is selected from water soluble nickel salt, for example one or more in nickelous nitrate, nickelous chloride, nickelous bromide, nickelous iodide and the single nickel salt.
The concentration of nickel salt aqueous solution is 0.05～3mol/L, is preferably 0.5～2mol/L.
The mol ratio of precipitation agent and nickel salt is 1: 1～3: 1.
Inorganic salt in the step (1) are preferably one or more in sodium-chlor, Repone K, sodium sulfate, vitriolate of tartar, sodium phosphate and the potassiumphosphate.
In the step (2), the mol ratio of inorganic salt and nickel oxide precursor is 0.1～2: 1, is preferably 0.2～1.2: 1.
In the step (2), drying temperature is 80～130 ℃, and be 6～8h time of drying; Maturing temperature is 300～600 ℃, and roasting time is 2～8h.
The present invention adopts inorganic salt to prevent that nickel oxide crystal grain and particulate sintering from growing up, and the grain fineness number of prepared nano nickel oxide is little, and resistance toheat is better.Method provided by the present invention has the advantages that technology is simple, easy to operate, production cost is low and environmental pollution is little, does not use tensio-active agent in its preparation process, and used inorganic salt are easy to reclaim.
Embodiment
Below further set forth the present invention through embodiment.
Embodiment 1
The nickel nitrate solution 50mL of preparation 1.2mol/L, the temperature to 70 of regulator solution ℃.The oxalic acid solution 100mL of the 0.6mol/L for preparing in advance is preheating to 70 ℃, oxalic acid solution is added in the nickel nitrate solution, produce the nickelous oxalate deposition in the solution at once.After continuing to stir 20min, in deposition, add the sodium chloride solution 50mL of 0.6mol/L, mixture is continued to be stirred to the moisture evaporate to dryness under 90 ℃.Powder at 450 ℃ of roasting 4h, obtains the pressed powder of blackish green behind 110 ℃ of oven dry 6h.With deionized water flush away sodium-chlor, obtain the nickel oxide pressed powder after 110 ℃ of oven dry.X-ray powder diffraction shows that this powder is the nickel oxide of pure phase.Wideization by the X-ray diffraction peak is 11nm through the mean grain size that the Scherrer formula calculates this nickel oxide, and the specific surface area that nitrogen adsorption method records nickel oxide is 94m
2/ g, pore volume are 0.34mL/g.
Embodiment 2
The nickel nitrate solution 50mL of preparation 1.2mol/L, the temperature to 70 of regulator solution ℃.The oxalic acid solution 100mL of the 0.6mol/L for preparing in advance is preheating to 70 ℃, oxalic acid solution is added in the nickel nitrate solution, produce the nickelous oxalate deposition in the solution at once.After continuing to stir 20min, in deposition, add the Klorvess Liquid 100mL of 0.6mol/L, mixture is continued to be stirred to the moisture evaporate to dryness under 80 ℃.Powder at 450 ℃ of roasting 4h, obtains the pressed powder of blackish green behind 110 ℃ of oven dry 6h.With deionized water flush away Repone K, obtain the nickel oxide pressed powder after 110 ℃ of oven dry.X-ray powder diffraction shows that this powder is the nickel oxide of pure phase.Wideization by the X-ray diffraction peak is 26nm through the mean grain size that the Scherrer formula calculates this nickel oxide, and the specific surface area that nitrogen adsorption method records nickel oxide is 32m
2/ g, pore volume are 0.22mL/g.
Comparative Examples 1
The nickel nitrate solution 50mL of preparation 1.2mol/L, the temperature to 70 of regulator solution ℃.The oxalic acid solution 100mL of the 0.6mol/L for preparing in advance is preheating to 70 ℃, oxalic acid solution is added in the nickel nitrate solution, produce the nickelous oxalate deposition in the solution at once.This is deposited in 70 ℃ continues aging 5h down.Deposition after 110 ℃ of oven dry, at 450 ℃ of roasting 4h, obtains the pressed powder of blackish green with the nickelous oxalate powder that obtains through filtration, deionized water wash, and X-ray powder diffraction shows that this powder is the nickel oxide of pure phase.Wideization by the X-ray diffraction peak is 77nm through the mean grain size that the Scherrer formula calculates this nickel oxide, and the specific surface area that nitrogen adsorption method records nickel oxide is 12m
2/ g, pore volume are 0.08mL/g.
Embodiment 3
The nickel nitrate solution 100mL of preparation 1.0mol/L, the temperature to 80 of regulator solution ℃.The sodium hydroxide solution 200mL of the 1.0mol/L for preparing in advance is preheating to 80 ℃, sodium hydroxide solution is added in the nickel nitrate solution, produce nickel hydroxide precipitate in the solution at once.Continue to be stirred to deposition fully after, with sedimentation and filtration, washing, powder obtains nickel hydroxide powder through 110 ℃ after drying 6h.Take by weighing 5.85g sodium-chlor, and ground behind the above-mentioned nickel hydroxide powder mixing that obtains 1 hour, again with mixture in 400 ℃ of roasting 6h.With the sodium-chlor in the deionized water flush away mixture, obtain the nickel oxide pressed powder after 110 ℃ of oven dry.X-ray powder diffraction shows that this powder is the nickel oxide of pure phase.Wideization by the X-ray diffraction peak is 18nm through the mean grain size that the Scherrer formula calculates this nickel oxide, and the specific surface area that nitrogen adsorption method records nickel oxide is 59m
2/ g, pore volume are 0.39mL/g.
Comparative Examples 2
The nickel nitrate solution 100mL of preparation 1.0mol/L, the temperature to 80 of regulator solution ℃.The sodium hydroxide solution 200mL of the 1.0mol/L for preparing in advance is preheating to 80 ℃, sodium hydroxide solution is added in the nickel nitrate solution, produce nickel hydroxide precipitate in the solution at once.Continue to be stirred to deposition fully after, with sedimentation and filtration, washing, powder obtains nickel hydroxide powder through 110 ℃ after drying 6h.Nickel hydroxide powder is obtained the nickel oxide pressed powder behind 400 ℃ of roasting 6h.X-ray powder diffraction shows that this powder is the nickel oxide of pure phase.Wideization by the X-ray diffraction peak is 32nm through the mean grain size that the Scherrer formula calculates this nickel oxide, and the specific surface area that nitrogen adsorption method records nickel oxide is 32m
2/ g, pore volume are 0.18mL/g.
Claims (14)
1. the preparation method of a nano-nickel oxide may further comprise the steps:
(1) with the precipitation agent aqueous solution and nickel salt aqueous solution reaction, generates deposition;
(2) inorganic salt with water soluble and heat decomposition temperature＞300 ℃ add in the system of steps (1), and evaporate to dryness water obtains mixture;
(3) with the mixture porphyrize of step (2), after drying, the roasting, washing obtains nano-nickel oxide through drying again;
Said precipitation agent is in water, to produce OH
-, CO
3 2-Or
-OOCCOO
-Material.
2. according to the described method of claim 1, it is characterized in that: the inorganic salt in the step (2) are selected from one or more in sodium-chlor, Repone K, sodium sulfate, vitriolate of tartar, sodium phosphate and the potassiumphosphate.
3. according to the described method of claim 1, it is characterized in that: the mol ratio of inorganic salt and nickel salt is 0.1～2: 1.
4. according to the described method of claim 3, it is characterized in that: the mol ratio of inorganic salt and nickel salt is 0.2～1.2: 1.
5. according to the described method of claim 1, it is characterized in that: precipitation agent is selected from one or more in ammoniacal liquor, urea, sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood, volatile salt, bicarbonate of ammonia, oxalic acid, sodium oxalate and the potassium oxalate.
6. according to the described method of claim 1, it is characterized in that: nickel salt is selected from one or more in nickelous nitrate, nickelous chloride, nickelous bromide, nickelous iodide and the single nickel salt.
7. according to the described method of claim 1, it is characterized in that: in the step (3), maturing temperature is 300～600 ℃, and roasting time is 2～8h.
8. the preparation method of a nano nickel oxide particles may further comprise the steps:
(1) with the precipitation agent aqueous solution and nickel salt aqueous solution reaction, generates deposition, after filtration, washing, drying, obtain the nickel oxide precursor powder;
(2) inorganic salt with the nickel oxide precursor powder of gained in the step (1) and water soluble and heat decomposition temperature＞300 ℃ mix, grinding, and roasting is washed, and obtains nano nickel oxide particles after the drying;
Said precipitation agent is in water, to produce OH
-, CO
3 2-Or
-OOCCOO
-Material.
9. according to the described method of claim 8, it is characterized in that: inorganic salt are one or more in sodium-chlor, Repone K, sodium sulfate, vitriolate of tartar, sodium phosphate and the potassiumphosphate.
10. according to the described method of claim 8, it is characterized in that: the mol ratio of inorganic salt and nickel oxide precursor powder is 0.1～2: 1.
11. according to the described method of claim 10, it is characterized in that: the mol ratio of inorganic salt and nickel oxide precursor powder is 0.2～1.2: 1.
12. according to the described method of claim 8, it is characterized in that: precipitation agent is selected from one or more in ammoniacal liquor, urea, sodium hydroxide, Pottasium Hydroxide, yellow soda ash, salt of wormwood, volatile salt, bicarbonate of ammonia, oxalic acid, sodium oxalate and the potassium oxalate.
13. according to the described method of claim 8, it is characterized in that: nickel salt is selected from one or more in nickelous nitrate, nickelous chloride, nickelous bromide, nickelous iodide and the single nickel salt.
14. according to the described method of claim 8, it is characterized in that: in the step (2), maturing temperature is 300～600 ℃, and roasting time is 2～8h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US11795555B2 (en) | 2018-02-23 | 2023-10-24 | King Fahd University Of Petroleum And Minerals | Method of making NiO nanoparticles for electrocatalytic water splitting |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102139931B (en) * | 2010-01-29 | 2012-08-01 | 中国石油化工股份有限公司 | Preparation method of nano nickel oxide |
| CN101863520B (en) * | 2010-06-17 | 2012-05-30 | 吉林市弗兰达科技股份有限公司 | Preparation method of microporous ultrafine high activity nickel carbonate |
| CN102154549B (en) * | 2011-02-21 | 2012-12-19 | 宇辰新能源材料科技无锡有限公司 | Production method for high-purity hard-agglomeration-free superfine nickel oxide or cobalt and nickel or cobalt powder |
| CN102757101B (en) * | 2012-02-22 | 2014-01-01 | 太原理工大学 | Method for preparing large-specific-surface-area porous nickel oxide microspheres |
| CN103333034A (en) * | 2013-06-27 | 2013-10-02 | 南京理工大学 | Nano nickel oxide coated modified boron fuel and preparation methods thereof |
| CN106098411B (en) * | 2016-06-29 | 2019-04-09 | 渤海大学 | A kind of preparation method of nickel oxide hierarchical organization material |
| CN106587176A (en) * | 2016-12-22 | 2017-04-26 | 太原理工大学 | Method for preparing super-small nickel hydroxide nanosheet by solution immersion method |
| CN106587175A (en) * | 2016-12-22 | 2017-04-26 | 太原理工大学 | Preparation method for electrode of ultra-small nickel hydroxide nanosheet |
| CN108285334A (en) * | 2018-01-26 | 2018-07-17 | 河海大学 | A kind of preparation method of nano oxidized Ni-Coated alumina powder body material |
| CN109455775B (en) * | 2018-11-27 | 2021-03-26 | 中南大学 | Preparation method of nano nickel oxide |
| CN109749516A (en) * | 2018-12-29 | 2019-05-14 | 武汉理工大学 | A kind of inkjet printing photochromic ceramic ink and preparation method thereof |
| CN110211813B (en) * | 2019-06-25 | 2021-05-14 | 中原工学院 | Rod-shaped nickel hydroxide electrode material, preparation method and super capacitor prepared from rod-shaped nickel hydroxide electrode material |
| CN113976122B (en) * | 2021-11-18 | 2023-11-03 | 四川启睿克科技有限公司 | NiO/Ni dual-function electrolytic water catalyst and preparation method thereof |
| CN115043445A (en) * | 2022-05-17 | 2022-09-13 | 华碧新能源技术研究(苏州)有限公司 | Preparation method and application of nickel oxide nanoparticles |
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| CN1948168A (en) * | 2006-10-31 | 2007-04-18 | 山东师范大学 | Synthesis method of nickel hydroxide nano-tube |
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| CN1948168A (en) * | 2006-10-31 | 2007-04-18 | 山东师范大学 | Synthesis method of nickel hydroxide nano-tube |
Non-Patent Citations (1)
| Title |
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| 李建芬等.均匀沉淀法制备纳米氧化镍的正交实验研究.《化工新型材料》.2008,第36卷(第1期),第51页. * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US11795555B2 (en) | 2018-02-23 | 2023-10-24 | King Fahd University Of Petroleum And Minerals | Method of making NiO nanoparticles for electrocatalytic water splitting |
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