CN104923804A - Preparation method of nickel nanoparticles - Google Patents
Preparation method of nickel nanoparticles Download PDFInfo
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- CN104923804A CN104923804A CN201510382583.3A CN201510382583A CN104923804A CN 104923804 A CN104923804 A CN 104923804A CN 201510382583 A CN201510382583 A CN 201510382583A CN 104923804 A CN104923804 A CN 104923804A
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Abstract
The invention belongs to the technical field of nanometer material synthesis, and particularly relates to a green and environment-friendly method for synthesizing nickel nanoparticles. The method includes the steps of adding acetylacetone nickel to olive oil, conducting heating to the temperature of 100 DEG C under the protection of nitrogen, keeping the temperature for 2 minutes, raising the temperature to 120 DEG C, keeping the temperature for 20 minutes, then raising the temperature to 260 DEG C to 280 DEG C, keeping the temperature for 10 minutes to 30 minutes, decreasing the temperature to 70 DEG C to 80 DEG C under the protection of nitrogen, cleaning obtained reaction liquid with n-butyl alcohol and normal hexane, and centrifugally separating out a product to obtain the nickel nanoparticles. The nickel nanoparticles prepared through a solvent thermal method are uniform in size, the production process is simple, the whole process is green and environmentally friendly, and no pollution can be caused to the environment.
Description
Technical field
The invention belongs to the technical field of nano material synthesis, the method for the synthesis nickel nano particle of particularly a kind of environmental protection.
Background technology
For a long time, magnetic Nano material relies on it at Magnetic resonance imaging, magnetic recording, electronics nano-device, drug delivery, catalyst, absorbing material, the wide application prospect in the fields such as high density information storage, thus paid close attention to widely, nickel nano particle has strong ferromagnetism, high surface, pore-free permeates, and specific area is large, there is the character that great skin effect and bulk effect etc. are unique, show the property corresponded to not available for body material.In recent years, owing to constantly increasing for the requirement of energy aspect in the world, so be badly in need of wanting development and exploration storage capacity outstanding, the battery technology that serviceability is stable, and nickel/metal and lithium ion battery just have these excellent character; Nickel nano particle can join in ballistite, significantly can increase the heat that fuel combustion produces, play the effect of good catalytic combustion efficiency, nickel becomes in the reaction of methyl alcohol at catalysis carbon dioxide reduction to play important catalytic action simultaneously, these all tool have very great significance, therefore, people have dropped into huge energy for the research of the synthetic method of nickel nano particle.
The existing method preparing nickel nano material has a variety of, as wet-chemical reducing process, and hydrogen reduction method, complexing displacement reducing process, solvent-thermal method etc., wherein hydrogen reduction method and complexing displacement reducing process productive rate low, production stage is loaded down with trivial details, and equipment requirement is high, is not easy to large-scale production; And wet-chemical reducing process although to have production technology simple, the advantage that product controllability is good, but usually need to use the reducing agent with strong reducing property in course of reaction, such as hydrazine, sodium borohydride etc., these materials itself have certain toxicity, can bring very large impact to the health of human body of ecological environment and user.Solvent-thermal method is a kind of new material preparation method grown up on the basis of hydro-thermal method, adopts and is similar to hydro-thermal ratio juris, can prepare cannot synthesize in aqueous, oxidizable, facile hydrolysis or the material to water sensitive.Compare compared to other preparation methods, the distinguishing feature of solvent-thermal process is: reaction is carried out in organic solvent, and this preparation for high purity material is very important: the target product that the employing of nonaqueous solvents makes solvent-thermal method to prepare increases greatly.Often the virose organic solvent of some tools also can be used in corresponding solvent thermal process, in use also must can cause environmental pollution, ecological environment is damaged, so have important practical significance for the research of the method for the synthesis nano nickel particles of environmental protection.
Therefore, probe into high efficiency and eco-friendly method synthesis nickel nano particle there is important academic significance and using value.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the shortcoming that background technology exists, and provides that a kind of technique is simple, the preparation method of nickel nano particle that environmental protection, Product size are homogeneous.
Technical problem of the present invention solves by the following technical programs:
A preparation method for nickel nano particle, adds nickel acetylacetonate in olive oil, and consumption is that every ml olive oil uses 0.08 ~ 0.12mmol nickel acetylacetonate; Under nitrogen protection, be heated to 100 DEG C with the heating rate of 10 DEG C per minute, constant temperature keeps 2 minutes, then temperature is risen to 120 DEG C, and heated at constant temperature is fully dissolved to nickel acetylacetonate for 20 minutes; Adjustment heating rate is 20 ~ 50 DEG C per minute, and be warming up to 260 ~ 280 DEG C, heated at constant temperature 10 ~ 30 minutes, lowers the temperature under nitrogen protection; By gained reactant liquor n-butanol and n-hexane cleaning, centrifugation product, obtains nano nickel particles, is dispersed in n-hexane and preserves.
Described cooling under nitrogen protection, is preferably cooled to 70 ~ 80 DEG C.This temperature is conducive to cleaning.
Described cleans with n-butanol and n-hexane, and can wash sample 4 ~ 5 times, wherein the volume ratio of n-hexane, n-butanol and reactant liquor is 1: 2: 1.
Beneficial effect:
1, the present invention's nano nickel particles size uniformity of adopting solvent-thermal method to prepare.
2, production technology of the present invention is simple, and the reagent of use all can be bought on the market, does not need to be further processed.
3, the present invention uses olive oil as solvent and reducing agent, does not add other any virose additives, whole process environmental protection, can not bring any pollution to environment.
Accompanying drawing illustrates:
Fig. 1 is the X ray diffracting spectrum of the nano nickel particles that embodiment 1 obtains.
Fig. 2 is the transmission electron microscope picture of the nano nickel particles that embodiment 1 obtains.
Fig. 3 is the X ray diffracting spectrum of the nano nickel particles that embodiment 2 obtains.
Fig. 4 is the X ray diffracting spectrum of the nano nickel particles that embodiment 3 obtains.
Fig. 5 is the X ray diffracting spectrum of the nano nickel particles that embodiment 4 obtains.
Fig. 6 is the X ray diffracting spectrum of the nano nickel particles that embodiment 5 obtains.
Fig. 7 is the X ray diffracting spectrum of the nano nickel particles that embodiment 6 obtains.
Fig. 8 is the X ray diffracting spectrum that embodiment 7 obtains nano nickel particles.
Detailed description of the invention:
In conjunction with elaboration the inventive method that following embodiment is more concrete, if no special instructions, agents useful for same is commercially available obtainable product, without the need to use of purifying further.
Embodiment 1: synthesis nano nickel particles
5ml olive oil and 0.4mmol nickel acetylacetonate is added in 50ml three-necked bottle, access nitrogen protection Xi Laike system, and with the heating of heating jacket temperature control under the state of magnetic agitation, first be heated to 100 DEG C with the heating rate of 10 DEG C per minute, keep 2 minutes, be warming up to 120 DEG C again, react 20 minutes, nickel acetylacetonate is fully dissolved; Then with 20 DEG C of heating rates per minute, temperature is risen to 280 DEG C, react 15 minutes; Nitrogen protection borehole cooling to 70 ~ 80 DEG C more afterwards; wash sample 4 ~ 5 times (wherein reactant liquor and n-hexane, the ratio of n-butanol is 1:1:2) with n-butanol and n-hexane, use centrifuge separated product; obtain black powder, it is dispersed in n-hexane and preserves.
The XRD collection of illustrative plates of the sample that the present embodiment obtains is as Fig. 1, and transmission electron microscope photo is shown in Fig. 2, and the product being characterized embodiment 1 by the XRD collection of illustrative plates of Fig. 1 is pure nickel nano particle.By the comparison with standard nickel XRD spectra, find to meet completely with card JCPDS 45-1027 (hexagonal phase) and JCPDS 87-0712 (Emission in Cubic).Wherein 39.1 °, 41.6 °, 44.5,58.4,78.0 corresponding hexagonal phase nickel 010}, and 002}, 011}, 012}, 103} crystal face, 44.5 °, 51.8 °, 76.4 ° of corresponding cubic-phase nickel of difference 111}, and 200}, 220} crystal face.
Embodiment 2: synthesize nano nickel particles by the mode reducing the reaction time
5ml olive oil and 0.4mmol nickel acetylacetonate is added in 50ml three-necked bottle, access nitrogen protection Xi Laike system, and with the heating of heating jacket temperature control under the state of magnetic agitation, first be heated to 100 DEG C with the heating rate of 10 DEG C per minute, keep 2 minutes, be warming up to 120 DEG C again, react 20 minutes, nickel acetylacetonate is fully dissolved; Then with 20 DEG C of heating rates per minute, temperature is risen to 280 DEG C, react 10 minutes; Nitrogen protection borehole cooling to 70 ~ 80 DEG C more afterwards; wash sample 4 ~ 5 times (wherein reactant liquor and n-hexane, the ratio of n-butanol is 1:1:2) with n-butanol and n-hexane, use centrifuge separated product; obtain black powder, it is dispersed in n-hexane and preserves.
The XRD collection of illustrative plates of the sample that the present embodiment obtains is as Fig. 3, and the product being characterized embodiment 2 by XRD collection of illustrative plates is pure nickel nano particle.By the comparison with standard nickel XRD spectra, find to meet completely with card JCPDS45-1027 (hexagonal phase) and JCPDS 87-0712 (Emission in Cubic).
Embodiment 3: synthesize nano nickel particles by the mode increasing the reaction time
5ml olive oil and 0.4mmol nickel acetylacetonate is added in 50ml three-necked bottle, access nitrogen protection Xi Laike system, and with the heating of heating jacket temperature control under the state of magnetic agitation, first be heated to 100 DEG C with the heating rate of 10 DEG C per minute, keep 2 minutes, be warming up to 120 DEG C again, react 20 minutes, nickel acetylacetonate is fully dissolved; Then with 20 DEG C of heating rates per minute, temperature is risen to 280 DEG C, react 30 minutes; Nitrogen protection borehole cooling to 70 ~ 80 DEG C more afterwards; wash sample 4 ~ 5 times (wherein reactant liquor and n-hexane, the ratio of n-butanol is 1:1:2) with n-butanol and n-hexane, use centrifuge separated product; obtain black powder, it is dispersed in n-hexane and preserves.
The XRD collection of illustrative plates of the sample that the present embodiment obtains, as Fig. 4, is the nano nickel particles of hexagonal phase and Emission in Cubic mixed phase by the product of XRD collection of illustrative plates sign embodiment 3.By the comparison with standard nickel XRD spectra, find to meet completely with card JCPDS 45-1027 (hexagonal phase) and JCPDS 87-0712 (Emission in Cubic).
Embodiment 4: the concentration synthesis nano nickel particles changing nickel source
5ml olive oil and 0.6mmol nickel acetylacetonate is added in 50ml three-necked bottle, access nitrogen protection Xi Laike system, and with the heating of heating jacket temperature control under the state of magnetic agitation, first be heated to 100 DEG C with the heating rate of 10 DEG C per minute, keep 2 minutes, be warming up to 120 DEG C again, react 20 minutes, nickel acetylacetonate is fully dissolved; Then with 20 DEG C of heating rates per minute, temperature is risen to 280 DEG C, react 30 minutes; Nitrogen protection borehole cooling to 70 ~ 80 DEG C more afterwards; wash sample 4 ~ 5 times (wherein reactant liquor and n-hexane, the ratio of n-butanol is 1:1:2) with n-butanol and n-hexane, use centrifuge separated product; obtain black powder, it is dispersed in n-hexane and preserves.
The XRD collection of illustrative plates of the sample that the present embodiment obtains, as Fig. 5, is the nano nickel particles of hexagonal phase and Emission in Cubic mixed phase by the product of XRD collection of illustrative plates sign embodiment 4.By the comparison with standard nickel XRD spectra, find to meet completely with card JCPDS 45-1027 (hexagonal phase) and JCPDS 87-0712 () Emission in Cubic.
Embodiment 5: the nano nickel particles that the mode changing reaction temperature is synthesized
5ml olive oil and 0.4mmol nickel acetylacetonate is added in 50ml three-necked bottle, access nitrogen protection Xi Laike system, and with the heating of heating jacket temperature control under the state of magnetic agitation, first be heated to 100 DEG C with the heating rate of 10 DEG C per minute, keep 2 minutes, be warming up to 120 DEG C again, react 20 minutes, nickel acetylacetonate is fully dissolved; Then with 20 DEG C of heating rates per minute, temperature is risen to 260 DEG C, react 30 minutes; Nitrogen protection borehole cooling to 70 ~ 80 DEG C more afterwards; wash sample 4 ~ 5 times (wherein reactant liquor and n-hexane, the ratio of n-butanol is 1:1:2) with n-butanol and n-hexane, use centrifuge separated product; obtain black powder, it is dispersed in n-hexane and preserves.
The XRD collection of illustrative plates of the sample that the present embodiment obtains is as Fig. 6, and the product being characterized embodiment 5 by XRD collection of illustrative plates is the nano nickel particles of Emission in Cubic.By the comparison with standard nickel XRD spectra, find to meet completely with card JCPDS87-0712 (Emission in Cubic).
By reducing reaction temperature, we obtain the nano nickel particles of Emission in Cubic, the nano nickel particles of what the first two example obtained is all hexagonal phase and Emission in Cubic mixed phase.
Embodiment 6: increase nickel source concentration under the reaction temperature of example 5, synthesis nano nickel particles
5ml olive oil and 0.6mmol nickel acetylacetonate is added in 50ml three-necked bottle, access nitrogen protection Xi Laike system, and with the heating of heating jacket temperature control under the state of magnetic agitation, first be heated to 100 DEG C with the heating rate of 10 DEG C per minute, keep 2 minutes, be warming up to 120 DEG C again, react 20 minutes, nickel acetylacetonate is fully dissolved; Then with 20 DEG C of heating rates per minute, temperature is risen to 260 DEG C, react 30 minutes; Nitrogen protection borehole cooling to 70 ~ 80 DEG C more afterwards; wash sample 4 ~ 5 times (wherein reactant liquor and n-hexane, the ratio of n-butanol is 1:1:2) with n-butanol and n-hexane, use centrifuge separated product; obtain black powder, it is dispersed in n-hexane and preserves.
The XRD collection of illustrative plates of the sample that the present embodiment obtains, as Fig. 7, is the nano nickel particles of hexagonal phase and Emission in Cubic mixed phase by the product of XRD collection of illustrative plates sign embodiment 6.By the comparison with standard nickel XRD spectra, find to meet completely with card JCPDS 45-1027 (hexagonal phase) and JCPDS 87-0712 () Emission in Cubic.
Embodiment 7: synthesize nano nickel particles by changing heating rate
5ml olive oil and 0.4mmol nickel acetylacetonate is added in 50ml three-necked bottle, access nitrogen protection Xi Laike system, and with the heating of heating jacket temperature control under the state of magnetic agitation, first be heated to 100 DEG C with the heating rate of 10 DEG C per minute, keep 2 minutes, be warming up to 120 DEG C again, react 20 minutes, nickel acetylacetonate is fully dissolved; Then with 20 DEG C of heating rates per minute, temperature is risen to 200 DEG C, then rise to 280 DEG C with the heating rate of 50 DEG C per minute; React 30 minutes; Nitrogen protection borehole cooling to 70 ~ 80 DEG C more afterwards; wash sample 4 ~ 5 times (wherein reactant liquor and n-hexane, the ratio of n-butanol is 1:1:2) with n-butanol and n-hexane, use centrifuge separated product; obtain black powder, it is dispersed in n-hexane and preserves.
The XRD collection of illustrative plates of the sample that the present embodiment obtains, as Fig. 8, is the nano nickel particles of hexagonal phase and Emission in Cubic mixed phase by the product of XRD collection of illustrative plates sign embodiment 7.By the comparison with standard nickel XRD spectra, find to meet completely with card JCPDS 45-1027 (hexagonal phase) and JCPDS 87-0712 (Emission in Cubic).
Claims (3)
1. a preparation method for nickel nano particle, adds nickel acetylacetonate in olive oil, and consumption is that every ml olive oil uses 0.08 ~ 0.12mmol nickel acetylacetonate; Under nitrogen protection, be heated to 100 DEG C with the heating rate of 10 DEG C per minute, constant temperature keeps 2 minutes, then temperature is risen to 120 DEG C, and heated at constant temperature is fully dissolved to nickel acetylacetonate for 20 minutes; Adjustment heating rate is 20 ~ 50 DEG C per minute, and be warming up to 260 ~ 280 DEG C, heated at constant temperature 10 ~ 30 minutes, lowers the temperature under nitrogen protection; By gained reactant liquor n-butanol and n-hexane cleaning, centrifugation product, obtains nano nickel particles, is dispersed in n-hexane and preserves.
2. according to the preparation method of nickel nano particle according to claim 1, it is characterized in that described cooling is under nitrogen protection cooled to 70 ~ 80 DEG C.
3. according to the preparation method of the nickel nano particle described in claim 1 or 2, it is characterized in that, described cleans with n-butanol and n-hexane, and be wash sample 4 ~ 5 times, wherein the volume ratio of n-hexane, n-butanol and reactant liquor is 1: 2: 1.
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| CN106607594A (en) * | 2016-11-30 | 2017-05-03 | 重庆文理学院 | Rapid low-cost preparation method of gold nanoparticles |
| CN106735297A (en) * | 2016-12-13 | 2017-05-31 | 哈尔滨商业大学 | The method that golden nanometer particle is prepared using maize germ oil |
| CN114769612A (en) * | 2022-04-24 | 2022-07-22 | 河南大学 | Oil-soluble nickel nano-particles, in-situ synthesis method thereof in vegetable oil and application thereof as vegetable oil anti-wear additive |
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| CN106735297A (en) * | 2016-12-13 | 2017-05-31 | 哈尔滨商业大学 | The method that golden nanometer particle is prepared using maize germ oil |
| CN114769612A (en) * | 2022-04-24 | 2022-07-22 | 河南大学 | Oil-soluble nickel nano-particles, in-situ synthesis method thereof in vegetable oil and application thereof as vegetable oil anti-wear additive |
| 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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