CN104923804B - A kind of preparation method of nickel nano particle - Google Patents
A kind of preparation method of nickel nano particle Download PDFInfo
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- CN104923804B CN104923804B CN201510382583.3A CN201510382583A CN104923804B CN 104923804 B CN104923804 B CN 104923804B CN 201510382583 A CN201510382583 A CN 201510382583A CN 104923804 B CN104923804 B CN 104923804B
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Abstract
The invention belongs to the technical field of nano material synthesis, the method for the synthesis nickel nano particle of more particularly to a kind of environmental protection.Nickel acetylacetonate is added in olive oil; then under nitrogen protection, 100 DEG C are heated to, constant temperature is kept for 2 minutes; then temperature is risen to 120 DEG C; heated at constant temperature 20 minutes, then it is warming up to 260 DEG C~280 DEG C, heated at constant temperature 10~30 minutes; 70~80 DEG C are cooled under nitrogen protection; gained reaction solution is cleaned with n-butanol and n-hexane, product is centrifuged, obtains nano nickel particles.The nano nickel particles size uniformity that the present invention is prepared using solvent-thermal method, simple production process, whole process environmental protection will not bring any pollution to environment.
Description
Technical field
The invention belongs to the technical field of nano material synthesis, the synthesis nickel nano particle of more particularly to a kind of environmental protection
Method.
Background technology
Since some time, magnetic Nano material by it in Magnetic resonance imaging, magnetic recording, electronics nano-device,
Drug delivery, catalyst, absorbing material, high density information storage etc. field wide application prospect so that by extensive
Concern, nickel nano particle has strong ferromagnetism, and high surface, pore-free infiltration, specific surface area is big, there is great skin effect
Unique property, shows the property corresponded to not available for body material with bulk effect etc..In recent years, due to the world
On be continuously increased for the requirement in terms of the energy, so be badly in need of want development and exploration storage capacity outstanding, performance stably electricity
Pool technology, and ni au category and lithium ion battery just have these excellent properties；Nickel nano particle can be added to rocket solid
In fuel, it can significantly increase the heat of fuel combustion generation, play a part of being catalyzed efficiency of combustion well, while nickel
In catalysis carbon dioxide reduction into important catalytic action is played in the reaction of methanol, these all have and had very great significance, because
This, people have put into huge energy for the research of the synthetic method of nickel nano particle.
The existing method for preparing nickel nano material has many kinds, such as wet-chemical reducing process, hydrogen reduction method, complexing displacement
Reducing process, solvent-thermal method etc., wherein hydrogen reduction method and complexing replaces reducing process low yield, and production stage is cumbersome, equipment requirement
Height, is not easy to large-scale production；Although and wet-chemical reducing process have simple production process, the good advantage of product controllability,
It is to usually require during the course of the reaction using the reducing agent with strong reducing property, such as hydrazine, sodium borohydride etc., these materials are in itself
With certain toxicity, very big influence can be brought to the health of human body of ecological environment and user.Solvent-thermal method is in hydro-thermal
A kind of new material preparation method grown up on the basis of method, using the principle similar to hydro-thermal method, can be prepared in water
Can not be synthesized in solution, oxidizable, facile hydrolysis or the material to water sensitive.Compared compared to other preparation methods, solvent heat seal
Into distinguishing feature be：Reaction is carried out in organic solvent, and this is very important for the preparation of high purity material：Non-aqueous
The target product that the use of agent causes solvent-thermal method and can prepared is greatly increased.Often it can also be used in corresponding solvent thermal process
Some have virose organic solvent, and environmental pollution is necessarily will also result in use, ecological environment is damaged, so right
There is important practical significance in the research of the method for the synthesis nano nickel particles of environmental protection.
Therefore, probe into high efficiency and environment-friendly method synthesis nickel nano particle has important academic significance and application
Value.
The content of the invention
The technical problem to be solved in the present invention is that the shortcoming for overcoming background technology to exist is simple, green there is provided a kind of technique
The preparation method of the homogeneous nickel nano particle of environmental protection, Product size.
The technical problem of the present invention is solved by the following technical programs：
A kind of preparation method of nickel nano particle, adds nickel acetylacetonate in olive oil, and consumption is to make per ml olive oil
With 0.08~0.12mmol nickel acetylacetonates；Under nitrogen protection, 100 DEG C, perseverance are heated to 10 DEG C per minute of heating rate
Temperature is kept for 2 minutes, temperature then is risen into 120 DEG C, heated at constant temperature fully dissolves for 20 minutes to nickel acetylacetonate；Adjustment heating speed
Rate is 20~50 DEG C per minute, is warming up to 260~280 DEG C, heated at constant temperature 10~30 minutes cools under nitrogen protection；By institute
Obtain reaction solution to be cleaned with n-butanol and n-hexane, centrifuge product, obtain nano nickel particles, be dispersed in n-hexane and preserve.
Described cooling under nitrogen protection, is preferably cooled to 70~80 DEG C.The temperature is conducive to cleaning.
Described is cleaned with n-butanol and n-hexane, can wash sample 4~5 times, wherein n-hexane, n-butanol and reaction solution
Volume ratio is 1: 2: 1.
Beneficial effect：
1st, the nano nickel particles size uniformity that the present invention is prepared using solvent-thermal method.
2nd, simple production process of the present invention, the reagent used can be bought on the market, it is not necessary to be further processed.
3rd, the present invention uses olive oil as solvent and reducing agent, without other any virose additives, entirely
Process environmental protection, will not bring any pollution to environment.
Brief description of the drawings:
Fig. 1 is the X ray diffracting spectrum for the nano nickel particles that embodiment 1 is obtained.
Fig. 2 is the transmission electron microscope picture of nano nickel particles made from embodiment 1.
Fig. 3 is the X ray diffracting spectrum of nano nickel particles made from embodiment 2.
Fig. 4 is the X ray diffracting spectrum of nano nickel particles made from embodiment 3.
Fig. 5 is the X ray diffracting spectrum of nano nickel particles made from embodiment 4.
Fig. 6 is the X ray diffracting spectrum of nano nickel particles made from embodiment 5.
Fig. 7 is the X ray diffracting spectrum of nano nickel particles made from embodiment 6.
Fig. 8 is the X ray diffracting spectrum that nano nickel particles are made in embodiment 7.
Embodiment：
With reference to the more specific elaboration the inventive method of following embodiment, unless otherwise specified, agents useful for same is city
Obtainable product is sold, is used without further purification.
Embodiment 1：Synthesize nano nickel particles
5ml olive oil and 0.4mmol nickel acetylacetonates, access nitrogen protection Xi Laike systems are added into 50ml three-necked bottles
System, and heated in the state of magnetic agitation with heating mantle temperature control, first it is heated to 100 with 10 DEG C per minute of heating rate
DEG C, kept for 2 minutes, then it is warming up to 120 DEG C, react 20 minutes, nickel acetylacetonate is fully dissolved；Then it is per minute with 20 DEG C
Heating rate, 280 DEG C are risen to by temperature, are reacted 15 minutes；Be cooled to 70~80 DEG C under nitrogen protection again afterwards, with n-butanol and
N-hexane washes sample 4~5 times, and (wherein reaction solution and n-hexane, the ratio of n-butanol is 1:1:2) centrifuge separation product, is used, is obtained
To black powder, it is dispersed in n-hexane and preserved.
The XRD spectrum of sample made from the present embodiment such as Fig. 1, transmission electron microscope photo is shown in Fig. 2, passes through Fig. 1 XRD stave
The product for levying embodiment 1 is pure nickel nano particle.By the comparison with standard nickel XRD spectra, find and card JCPDS 45-
1027 (hexagonal phases) and JCPDS 87-0712 (Emission in Cubic) are complied fully with.Wherein 39.1 °, 41.6 °, 44.5,58.4,78.0 pairs
Answer { 010 } of hexagonal phase nickel, { 002 }, { 011 }, { 012 }, { 103 } crystal face, 44.5 °, 51.8 °, 76.4 ° correspond to Emission in Cubic respectively
{ 111 } of nickel, { 200 }, { 220 } crystal face,.
Embodiment 2：Nano nickel particles are synthesized by way of reducing the reaction time
5ml olive oil and 0.4mmol nickel acetylacetonates, access nitrogen protection Xi Laike systems are added into 50ml three-necked bottles
System, and heated in the state of magnetic agitation with heating mantle temperature control, first it is heated to 100 with 10 DEG C per minute of heating rate
DEG C, kept for 2 minutes, then it is warming up to 120 DEG C, react 20 minutes, nickel acetylacetonate is fully dissolved；Then it is per minute with 20 DEG C
Heating rate, 280 DEG C are risen to by temperature, are reacted 10 minutes；Be cooled to 70~80 DEG C under nitrogen protection again afterwards, with n-butanol and
N-hexane washes sample 4~5 times, and (wherein reaction solution and n-hexane, the ratio of n-butanol is 1:1:2) centrifuge separation product, is used, is obtained
To black powder, it is dispersed in n-hexane and preserved.
The XRD spectrum of sample made from the present embodiment such as Fig. 3, the product for characterizing embodiment 2 by XRD spectrum is pure nickel
Nano particle.By the comparison with standard nickel XRD spectra, find and card JCPDS45-1027 (hexagonal phase) and JCPDS 87-
0712 (Emission in Cubic) is complied fully with.
Embodiment 3：Nano nickel particles are synthesized by way of increasing the reaction time
5ml olive oil and 0.4mmol nickel acetylacetonates, access nitrogen protection Xi Laike systems are added into 50ml three-necked bottles
System, and heated in the state of magnetic agitation with heating mantle temperature control, first it is heated to 100 with 10 DEG C per minute of heating rate
DEG C, kept for 2 minutes, then it is warming up to 120 DEG C, react 20 minutes, nickel acetylacetonate is fully dissolved；Then it is per minute with 20 DEG C
Heating rate, 280 DEG C are risen to by temperature, are reacted 30 minutes；Be cooled to 70~80 DEG C under nitrogen protection again afterwards, with n-butanol and
N-hexane washes sample 4~5 times, and (wherein reaction solution and n-hexane, the ratio of n-butanol is 1:1:2) centrifuge separation product, is used, is obtained
To black powder, it is dispersed in n-hexane and preserved.
The XRD spectrum of sample made from the present embodiment such as Fig. 4, the product for characterizing embodiment 3 by XRD spectrum is hexagonal phase
With the nano nickel particles of Emission in Cubic mixed phase.By the comparison with standard nickel XRD spectra, find and card JCPDS 45-1027 (six
Angle phase) and JCPDS 87-0712 (Emission in Cubic) comply fully with.
Embodiment 4：Change the concentration synthesis nano nickel particles of nickel source
5ml olive oil and 0.6mmol nickel acetylacetonates, access nitrogen protection Xi Laike systems are added into 50ml three-necked bottles
System, and heated in the state of magnetic agitation with heating mantle temperature control, first it is heated to 100 with 10 DEG C per minute of heating rate
DEG C, kept for 2 minutes, then it is warming up to 120 DEG C, react 20 minutes, nickel acetylacetonate is fully dissolved；Then it is per minute with 20 DEG C
Heating rate, 280 DEG C are risen to by temperature, are reacted 30 minutes；Be cooled to 70~80 DEG C under nitrogen protection again afterwards, with n-butanol and
N-hexane washes sample 4~5 times, and (wherein reaction solution and n-hexane, the ratio of n-butanol is 1:1:2) centrifuge separation product, is used, is obtained
To black powder, it is dispersed in n-hexane and preserved.
The XRD spectrum of sample made from the present embodiment such as Fig. 5, the product for characterizing embodiment 4 by XRD spectrum is hexagonal
Mutually with the nano nickel particles of Emission in Cubic mixed phase.By the comparison with standard nickel XRD spectra, find and card JCPDS 45-1027
(hexagonal phase) and JCPDS 87-0712 () Emission in Cubic is complied fully with.
Embodiment 5：Change the nano nickel particles that the mode of reaction temperature is synthesized
5ml olive oil and 0.4mmol nickel acetylacetonates, access nitrogen protection Xi Laike systems are added into 50ml three-necked bottles
System, and heated in the state of magnetic agitation with heating mantle temperature control, first it is heated to 100 with 10 DEG C per minute of heating rate
DEG C, kept for 2 minutes, then it is warming up to 120 DEG C, react 20 minutes, nickel acetylacetonate is fully dissolved；Then it is per minute with 20 DEG C
Heating rate, 260 DEG C are risen to by temperature, are reacted 30 minutes；Be cooled to 70~80 DEG C under nitrogen protection again afterwards, with n-butanol and
N-hexane washes sample 4~5 times, and (wherein reaction solution and n-hexane, the ratio of n-butanol is 1:1:2) centrifuge separation product, is used, is obtained
To black powder, it is dispersed in n-hexane and preserved.
The XRD spectrum of sample made from the present embodiment such as Fig. 6, by XRD spectrum characterize embodiment 5 product for cube
The nano nickel particles of phase.By the comparison with standard nickel XRD spectra, find to accord with completely with card JCPDS87-0712 (Emission in Cubic)
Close.
By reducing reaction temperature, we have obtained the nano nickel particles of Emission in Cubic, and what the first two example was obtained is all six
The nano nickel particles of angle phase and Emission in Cubic mixed phase.
Embodiment 6：Increase nickel source concentration under the reaction temperature of example 5, synthesize nano nickel particles
5ml olive oil and 0.6mmol nickel acetylacetonates, access nitrogen protection Xi Laike systems are added into 50ml three-necked bottles
System, and heated in the state of magnetic agitation with heating mantle temperature control, first it is heated to 100 with 10 DEG C per minute of heating rate
DEG C, kept for 2 minutes, then it is warming up to 120 DEG C, react 20 minutes, nickel acetylacetonate is fully dissolved；Then it is per minute with 20 DEG C
Heating rate, 260 DEG C are risen to by temperature, are reacted 30 minutes；Be cooled to 70~80 DEG C under nitrogen protection again afterwards, with n-butanol and
N-hexane washes sample 4~5 times, and (wherein reaction solution and n-hexane, the ratio of n-butanol is 1:1:2) centrifuge separation product, is used, is obtained
To black powder, it is dispersed in n-hexane and preserved.
The XRD spectrum of sample made from the present embodiment such as Fig. 7, the product for characterizing embodiment 6 by XRD spectrum is hexagonal
Mutually with the nano nickel particles of Emission in Cubic mixed phase.By the comparison with standard nickel XRD spectra, find and card JCPDS 45-1027
(hexagonal phase) and JCPDS 87-0712 () Emission in Cubic is complied fully with.
Embodiment 7：Nano nickel particles are synthesized by changing heating rate
5ml olive oil and 0.4mmol nickel acetylacetonates, access nitrogen protection Xi Laike systems are added into 50ml three-necked bottles
System, and heated in the state of magnetic agitation with heating mantle temperature control, first it is heated to 100 with 10 DEG C per minute of heating rate
DEG C, kept for 2 minutes, then it is warming up to 120 DEG C, react 20 minutes, nickel acetylacetonate is fully dissolved；Then it is per minute with 20 DEG C
Heating rate, rises to 200 DEG C, then rise to 280 DEG C with 50 DEG C per minute of heating rate by temperature；Reaction 30 minutes；Afterwards again
70~80 DEG C are cooled under nitrogen protection, sample is washed with n-butanol and n-hexane 4~5 times (wherein reaction solution and n-hexane, n-butanol
Ratio be 1:1:2) centrifuge separation product, is used, black powder is obtained, it is dispersed in n-hexane and preserved.
The XRD spectrum of sample made from the present embodiment such as Fig. 8, the product for characterizing embodiment 7 by XRD spectrum is hexagonal
Mutually with the nano nickel particles of Emission in Cubic mixed phase.By the comparison with standard nickel XRD spectra, find and card JCPDS 45-1027
(hexagonal phase) and JCPDS 87-0712 (Emission in Cubic) are complied fully with.
Claims (1)
1. a kind of preparation method of nickel nano particle, adds nickel acetylacetonate in olive oil, consumption is to be used per ml olive oil
0.08~0.12mmol nickel acetylacetonates；Under nitrogen protection, 100 DEG C, constant temperature are heated to 10 DEG C per minute of heating rate
Kept for 2 minutes, temperature is then risen to 120 DEG C, heated at constant temperature fully dissolves for 20 minutes to nickel acetylacetonate；Adjust heating rate
For 20~50 DEG C per minute, 260~280 DEG C are warming up to, heated at constant temperature 10~30 minutes cools under nitrogen protection；By gained
Reaction solution is cleaned with n-butanol and n-hexane, is centrifuged product, is obtained nano nickel particles, is dispersed in n-hexane and is preserved.
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| CN106607594B (en) * | 2016-11-30 | 2018-07-10 | 重庆文理学院 | A kind of quick, low cost gold nanoparticle preparation method |
| CN106735297B (en) * | 2016-12-13 | 2018-09-25 | 哈尔滨商业大学 | The method for preparing gold nanoparticle using maize germ oil |
| CN114769612B (en) * | 2022-04-24 | 2024-04-12 | 河南大学 | Oil-soluble nickel nano-particles, in-situ synthesis method of oil-soluble nickel nano-particles in vegetable oil and application of oil-soluble nickel nano-particles as vegetable oil antiwear additive |
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| CN101168196B (en) * | 2006-10-27 | 2010-09-15 | 同济大学 | Method for preparing nickel-base amorphous nano particles |
| CA2728987C (en) * | 2008-05-16 | 2018-12-04 | Verutek Technologies, Inc. | Green synthesis of nanometals using plant extracts and use thereof |
| CN101486451B (en) * | 2009-02-24 | 2012-01-25 | 中国科学院长春应用化学研究所 | Green method for synthesizing appearance and size controllable semiconductor nanocrystalline |
| CN101693297B (en) * | 2009-10-16 | 2011-06-08 | 厦门大学 | Preparation method of copper nanoparticles with different particle diameters |
| CN102616748B (en) * | 2012-04-11 | 2013-10-23 | 吉林大学 | Method for preparing nanometer metallic oxide by bulk metallic oxide |
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| CN102837004B (en) * | 2012-09-25 | 2015-02-04 | 吉林大学 | Preparation method of polyhedral copper nanoparticle |
| CN103194616B (en) * | 2013-04-08 | 2014-07-30 | 吉林大学 | Method for preparing copper nanocrystalline |
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