CN100448574C - Method for preparing nano nickel - Google Patents
Method for preparing nano nickel Download PDFInfo
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- CN100448574C CN100448574C CNB2005100946048A CN200510094604A CN100448574C CN 100448574 C CN100448574 C CN 100448574C CN B2005100946048 A CNB2005100946048 A CN B2005100946048A CN 200510094604 A CN200510094604 A CN 200510094604A CN 100448574 C CN100448574 C CN 100448574C
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Abstract
The present invention relates to a method for preparing nanometer nickel in different shapes. Nonionic surface active agents of a Tween series or a polyethylene glycol (PEG) series or respective compounds of the Tween series or the polyethylene glycol (PEG) and sodium dodecyl sulfate (SDS) are used as modifiers to be added to a nickel acetate solution, wherein the molar ratio of the modifiers and the nickel acetate is (1 to 2.5): 1, and the solution is dripped in a NaOH solution at a speed of 20 to 50 droplet/minute to regulate the pH value of the NaOH solution to be from 8 to 12. After dripping finishes, the solution is heated at a speed of 10 to 15 DEG C/minute for dehydration, is heated to more than 180 DEGC to carry out reactions for 0.2 to 0.5 h and is cooled down. 20 to 30 mL of propanone is added, and mixtures are centrifugally separated and are washed by the propanone and water to obtain the nanometer nickel in different shapes. The particle size of the nanometer nickel particles prepared by the method is from 26 to 180 nanometers, and the method has the advantages of environmental protection, mild reaction conditions, easy reaction control, low cost and simple and convenient process and process flow.
Description
Technical field
The present invention relates to preparation method of nano material, refer in particular to the nickel acetate is that raw material, polyalcohol are solvent and reducing agent, with non-ionic surfactant Tween (Tween) series or polyethylene glycol (PEG) series or they and the composite of lauryl sodium sulfate (SDS) is dressing agent, and the liquid phase chemical reduction legal system is equipped with the method for nanometer nickel.
Background technology
257) and J.Nanopartiele Research (7 (2005): statement is just arranged 51) crystallite dimension of nano metal material and pattern, surface state and micro-structural directly have influence on the physico-chemical property and the purposes of nano metal, are published in J.Catal (173 (1998): respectively as R.Molina, W.H.Qi etc.The nanostructured system is the research focus of current metal nano material, and the key of this research work just is to obtain pattern, granularity, the controlled nano-metal particle of structure.Nanometer nickel has unique physicochemical properties, has broad application prospects at aspects such as catalyst, magnetic material, sintering activator, electrocondution slurry, coating material, battery, carbide alloy binding agent, kollags.In preparation nanometer nickel, dressing agent commonly used is a polyelectrolyte class material, and prepared nanometer nickel mostly is the particle of sphere or class sphere, the cost height, course of reaction has certain toxicity, and environment is had pollution, is unfavorable for forming the nanometer nickel of different-shape, granularity, structure; And reaction precursor body or parent initial concentration are very low mostly, and products therefrom is less, and post processing is difficult, are unfavorable for carrying out the physical and chemical performance of follow-up study product and the application of expanding product.Concrete visible H.G.Zheng etc. is published in " Preparation of nickel nanopowders inethanol-water system (EWS) " on the Materials Research Bulletin and Y Hou etc. and is published in " Size-controlledsynthesis of nickel nanoparticles " on the Applied Surface Science etc.By retrieval, do not have as yet at present and utilize non-ionic surface active agent Tween series separately or composite for dressing agent prepares the report of nanometer nickel with SDS, PEG series separately or with also the reporting of the composite nanometer nickel for preparing multiple pattern, structure for dressing agent of SDS.
Summary of the invention
The present invention proposes a kind of is raw material with the nickel acetate, polyalcohol is solvent and reducing agent, composite with non-ionic surfactant Tween (Tween) series or polyethylene glycol (PEG) series or they and lauryl sodium sulfate (SDS) is dressing agent, liquid phase reduction prepares the method for nanometer nickel, to overcome above-mentioned shortcoming, and prepared nanometer nickel has multiple pattern, the micro-structural of size, these micro-structurals will have the physical and chemical performance of characteristic separately, can be the follow-up study different size, the application of the physical and chemical performance of pattern nanometer nickel and expansion nanometer nickel provides technical guarantee.
Its preparation method is as follows:
With 1, the 2-propane diols is a solvent, the nickel acetate solution of preparation 0.2～0.4mol/L, with non-ionic surfactant Tween (Tween) series or polyethylene glycol (PEG) series or they is that dressing agent joins in the nickel acetate solution with the composite of lauryl sodium sulfate (SDS) respectively, compound proportion is 1: 1, the mol ratio of dressing agent and nickel acetate is 1～2.5: 1, speed with 20～50/min splashes into the pH value of NaOH solution regulator solution between 8～12 again, after dropwising, speed intensification dehydration with 10～15 ℃/min, to reacting 0.2～0.5h more than 180 ℃, cooling adds 20～30mL acetone and disperses centrifugation, use acetone, water washing promptly gets the nanometer nickel of different-shape.
Above-mentioned preparation method, it is good should adopting following technological parameter or step:
With 1, the 2-propane diols is a solvent, the nickel acetate solution of preparation 0.3mol/L, the dressing agent that adds and the mol ratio of nickel acetate are 2～2.5: l, speed with 20～30/min splashes into the pH value of NaOH solution regulator solution between 10～12 again, after dropwising,, between 180 ℃～190 ℃, react 0.2～0.3h with the speed intensification dehydration of 13～15 ℃/min.
The dressing agent that uses is: Tween-20, Tween-40, Tween-80, PEG-200, PEG-600, PEG-2000, PEG-6000, Tween-20+SDS, Tween-40+SDS, Tween-80+SDS, PEG-200+SDS, PEG-600+SDS, PEG-2000+SDS or PEG-6000+SDS.
Description of drawings
Fig. 1: Tween-20 is the transmission electron microscope picture of the nanometer nickel product of dressing agent
Fig. 2: Tween-80 is the transmission electron microscope picture of the nanometer nickel product of dressing agent
Fig. 3: PEG-200 is the transmission electron microscope picture of the nanometer nickel product of dressing agent
Fig. 4: PEG-6000 is the transmission electron microscope picture of the nanometer nickel product of dressing agent
Fig. 5: SDS+Tween-40 is the transmission electron microscope picture of the nanometer nickel product of dressing agent
Fig. 6: SDS+PEG-200 is the transmission electron microscope picture of the nanometer nickel product of dressing agent
Fig. 7: SDS+PEG-2000 is the transmission electron microscope picture of the nanometer nickel product of dressing agent
Fig. 8: Tween-20 is the local SEAD figure of the nanometer nickel product of dressing agent
Fig. 9: SDS+PEG-2000 is the local SEAD figure of the nanometer nickel product of dressing agent
The specific embodiment
The present invention will be further described below in conjunction with concrete embodiment.
Embodiment 1
As Fig. 1, Fig. 8, take by weighing the nickel acetate of 2.4886g, be dissolved in 50mL 1, in the 2-propane diols,, add the Tween-20 of 0.04mol with this solution heating, stirring.Speed with 20/min splashes into the sodium hydroxide solution that concentration is 1.0mol/L, and regulating the pH value is 10.After dropwising, the speed intensification dehydration with 10 ℃/min is warming up to more than 180 ℃ again and reacts 0.2h, distills out most of solvent, is cooled to 50 ℃ again, adds 20mL acetone and disperses, and centrifugation with acetone, water washing, obtains nanometer nickel.
Embodiment 2
As Fig. 2, take by weighing the nickel acetate of 3.7329g, be dissolved in 50mL 1, in the 2-propane diols,, add the Tween-80 of 0.02mol with this solution heating, stirring.Speed with 30/min splashes into the sodium hydroxide solution that concentration is 1.0mol/L, regulates pH value 8.After dropwising, the speed intensification dehydration with 15 ℃/min is warming up to more than 180 ℃ again and reacts 0.3h, distills out most of solvent, is cooled to 50 ℃ again, adds 20mL acetone and disperses, and centrifugation with acetone, water washing, obtains the nanometer nickel of different-shape.
Embodiment 3
As Fig. 3, take by weighing the nickel acetate of 4.9772g, be dissolved in 50mL 1, in the 2-propane diols,, add the PEG-200 of 0.10mol with this solution heating, stirring.Speed with 50/min splashes into the sodium hydroxide solution that concentration is 1.0mol/L again, regulates pH value 12.After dropwising, the speed intensification dehydration with 10 ℃/min is warming up to more than 180 ℃ again and reacts 0.5h, distills out most of solvent, is cooled to 50 ℃ again, adds 30mL acetone and disperses, and centrifugation with acetone, water washing, obtains nanometer nickel.
Embodiment 4
As Fig. 4, take by weighing the nickel acetate of 2.4886g, be dissolved in 50mL 1, in the 2-propane diols,, add the PEG-6000 of 0.03mol with this solution heating, stirring.Speed with 30/min splashes into the sodium hydroxide solution that concentration is 1.0mol/L again, regulates pH value 10.After dropwising, the speed intensification dehydration with 15 ℃/min is warming up to more than 180 ℃ again and reacts 0.2h, distills out most of solvent, is cooled to 50 ℃ again, adds 20mL acetone and disperses, and centrifugation with acetone, water washing, obtains nanometer nickel.
Embodiment 5
As Fig. 5, take by weighing the nickel acetate of 2.4886g, be dissolved in 50mL 1, in the 2-propane diols,, add the Tween-80 of 0.01mol and the SDS of 0.01mol with this solution heating, stirring.Speed with 25/min splashes into the sodium hydroxide solution that concentration is 1.0mol/L again, regulates pH value 12.After dropwising, the speed intensification dehydration with 10 ℃/min is warming up to more than 180 ℃ again and reacts 0.5h, distills out most of solvent, is cooled to 50 ℃ again, adds 25mL acetone and disperses, and centrifugation with acetone, water washing, obtains nanometer nickel.
Embodiment 6
As Fig. 6, take by weighing the nickel acetate of 2.4886g, be dissolved in 50mL 1, in the 2-propane diols,, add the PEG-200 of 0.01mol and the SDS of 0.01mol with this solution heating, stirring.Speed with 25/min splashes into the sodium hydroxide solution that concentration is 1.0mol/L again, regulates pH value 10.After dropwising, the speed intensification dehydration with 10 ℃/min is warming up to more than 180 ℃ again and reacts 0.4h, distills out most of solvent, is cooled to 50 ℃ again, adds 30mL acetone and disperses, and centrifugation with acetone, water washing, obtains nanometer nickel.
Embodiment 7
As Fig. 7, Fig. 9, take by weighing the nickel acetate of 4.9772g, be dissolved in 50mL 1, in the 2-propane diols,, add the PEG-2000 of 0.02mol and the SDS of 0.02mol with this solution heating, stirring.Speed with 20/min splashes into the sodium hydroxide solution that concentration is 1.0mol/L again, regulates pH value 12.After dropwising, the speed intensification dehydration with 10 ℃/min is warming up to more than 180 ℃ again and reacts 0.5h, distills out most of solvent, is cooled to 50 ℃ again, adds 30mL acetone and disperses, and centrifugation with acetone, water washing, obtains nanometer nickel.
Table 1, table 2 are that different-shape, particle diameter, the particle diameter of part nanometer nickel distributes and ratio.
The particle diameter of table 1 different-shape nano nickel, particle diameter distribute and ratio
The particle diameter of table 2 different-shape nano nickel, particle diameter distribute and ratio
Claims (4)
1, a kind of method for preparing nanometer nickel, it is characterized in that: with 1, the 2-propane diols is a solvent, the nickel acetate solution of preparation 0.2～0.4mol/L, with non-ionic surfactant Tween (Tween) series or polyethylene glycol (PEG) series or they is that dressing agent joins in the nickel acetate solution with the composite of lauryl sodium sulfate (SDS) respectively, the mol ratio of dressing agent and nickel acetate is 1～2.5: 1, speed with 20～50/min splashes into the pH value of NaOH solution regulator solution between 8～12 again, after dropwising, speed intensification dehydration with 10～15 ℃/min, to reacting 0.2～0.5h more than 180 ℃, cooling adds 20～30mL acetone and disperses centrifugation, use acetone, water washing promptly gets the nanometer nickel of different-shape.
2, a kind of method for preparing nanometer nickel according to claim 1 is characterized in that: tween (Tween) series or polyethylene glycol (PEG) series are 1: 1 with the compound proportion of lauryl sodium sulfate (SDS).
3, according to claim 1 or the described a kind of method for preparing nanometer nickel of claim 2, it is characterized in that: the dressing agent of use is: Tween-20, Tween-40, Tween-80, PEG-200, PEG-600, PEG-2000, PEG-6000, Tween-20+SDS, Tween-40+SDS, Tween-80+SDS, PEG-200+SDS, PEG-600+SDS, PEG-2000+SDS or PEG-6000+SDS.
4, a kind of method for preparing nanometer nickel according to claim 1, it is characterized in that: with 1, the 2-propane diols is a solvent, the nickel acetate solution of preparation 0.3mol/L, the dressing agent that adds and the mol ratio of nickel acetate are 2～2.5: 1, and the pH value that splashes into NaOH solution regulator solution with the speed of 20～30/min is between 10～12, after dropwising again, with the speed intensification dehydration of 13～15 ℃/min, between 180 ℃～190 ℃, react 0.2～0.3h.
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| CN103374346A (en) * | 2012-04-13 | 2013-10-30 | 中国科学院高能物理研究所 | Method for improving water solubility of nanomaterial through surface modification and nanomaterial modified by method |
| CN106735304B (en) * | 2017-01-06 | 2018-11-09 | 西南科技大学 | Metal nano preparation of sections method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1223919A (en) * | 1998-12-29 | 1999-07-28 | 成都开飞高能化学工业有限公司 | Method for producing superfine sphere metallic nickel powder |
| WO2003031323A1 (en) * | 2001-10-12 | 2003-04-17 | Korea Nano Technology Co., Ltd. | Synthesis of mono-disperse and highly-crystalline nano-particles of metals, alloys, metal oxides, and multi-metallic oxides without a size-selection process |
| CN1586773A (en) * | 2004-08-06 | 2005-03-02 | 中山大学 | Nano structure nickel powde and its preparing method |
| US6878184B1 (en) * | 2002-08-09 | 2005-04-12 | Kovio, Inc. | Nanoparticle synthesis and the formation of inks therefrom |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1223919A (en) * | 1998-12-29 | 1999-07-28 | 成都开飞高能化学工业有限公司 | Method for producing superfine sphere metallic nickel powder |
| WO2003031323A1 (en) * | 2001-10-12 | 2003-04-17 | Korea Nano Technology Co., Ltd. | Synthesis of mono-disperse and highly-crystalline nano-particles of metals, alloys, metal oxides, and multi-metallic oxides without a size-selection process |
| US6878184B1 (en) * | 2002-08-09 | 2005-04-12 | Kovio, Inc. | Nanoparticle synthesis and the formation of inks therefrom |
| CN1586773A (en) * | 2004-08-06 | 2005-03-02 | 中山大学 | Nano structure nickel powde and its preparing method |
Non-Patent Citations (4)
| Title |
|---|
| 1，2-丙二醇液相还原法制备纳米镍粉的研究. 李鹏，官建国，张清杰，赵文俞，袁润章.材料科学与工艺，第9卷第3期. 2001 |
| 1，2-丙二醇液相还原法制备纳米镍粉的研究. 李鹏，官建国，张清杰，赵文俞，袁润章.材料科学与工艺，第9卷第3期. 2001 * |
| 超细镍粉的制备进展. 牛明勤，吴介达.精细化工，第20卷第12期. 2003 |
| 超细镍粉的制备进展. 牛明勤，吴介达.精细化工，第20卷第12期. 2003 * |
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