CN103706804A - Environment-friendly preparing method of nickel nanocrystalline - Google Patents
Environment-friendly preparing method of nickel nanocrystalline Download PDFInfo
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- CN103706804A CN103706804A CN201310725062.4A CN201310725062A CN103706804A CN 103706804 A CN103706804 A CN 103706804A CN 201310725062 A CN201310725062 A CN 201310725062A CN 103706804 A CN103706804 A CN 103706804A
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Abstract
Provided is an environment-friendly preparing method of nickel nanocrystalline. The preparing method comprises the following steps that first, nickel acetate tetrahydrate, sodium borohydride, choline chloride and urea are mixed together according to the mass ratio of 2:1:6:6, and are completely ground to be used; second, the above mixture is placed in a reaction kettle which is washed cleanly to be heated to 140-160 DEG C, and heat insulation is conducted for 4-6h; third, the reacted mixture is cleaned, filtered and dried so that nano nickel crystal particles which are high in purification, even in particle and good in dispersity, and have the average particle diameter being within 10-20nm are obtained. According to the environment-friendly preparing method of the nickel nanocrystalline, the pollution-free sodium borohydride is used as a reductive agent, the urea and the choline chloride which can be completely recycled are used as fused salt media, the process is simple, the method is safe and free of pollution, energy and time are saved, and great industrial application value is achieved.
Description
Technical field
The present invention relates to the preparation method of nanocrystal, relate in particular to the nanocrystalline environment-friendly preparation method thereof of a kind of nickel.
Background technology
Along with the quickening of world industry process, many scarce resources are all considered as strategic materials by every country, especially transition metal.Nickel is due to the property of itself, in fields such as electricity, magnetic, heat, there is important application very, with regard to its use consumption at catalytic field, in 2011, just break through 5000 tons, and the nickel powder manufacturing enterprise that China has is now considerably less, production capacity far can not meet domestic current use amount, needs a large amount of imports.The very wide electric bicycle of current domestic use face is used Ni-MH battery in a large number, it is raw material at micron-sized nickel that Ni-MH battery mainly be take particle size, because particle diameter is larger, can not give full play to the ability of Ni-MH battery, the flying power of electric bicycle can not be had greatly improved, if the particle of nickel can be accomplished nanoscale, under the small-size effect of nano material and the effect of skin effect, the specific area of nickel that participates in reaction increases by 9 orders of magnitude during than micron level, so not only increased the power of Ni-MH battery, simultaneously in the situation that battery capacity is constant, also make the volume and weight of Ni-MH battery greatly reduce, this capacity is large, volume is little, lightweight, the Ni-MH battery that flying power is strong will have the purposes of more crossing on market, even be sold abroad.Nanoscale nickel powder, owing to having great bulk effect and skin effect, makes it at aspects such as magnetic, interior pressure, thermal resistance, light absorption, chemisms, show many properties, as a kind of new material, more and more attracts widespread attention.Nano-nickel powder replaces common nickel powder as the catalyst of ballistite, to make fuel efficiency double, the particle diameter of take is less than the catalyst that the extra-fine nickel powder of 0.5 μ m is made as main component, the efficiency of its organic matter hydrogenation is ten times that traditional nickel is made catalyst, the light sintered body of extra-fine nickel powder can be made millipore filter, its average pore size can reach 10 nanometers, this nanometer micropore filter can be used for gas isotope, mixes the separated and concentrated of rare gas, organic compound, also can be for fermentation, medicine and biomaterial science.At present, the preparation of nickel powder, roughly there is following several method (1) carbonyl nickel thermal decomposition method at home and abroad, there is more serious shortcoming in this method, and the one, along with the rising of decomposition temperature in pyrolysis tower, the easy sintering of nickel powder, and granularity increases, the 2nd, carbonyl nickel is a kind of extremely toxic substance, hinders health, and environment is existed to serious pollution.(2) electrolysis adds Ni in electrolytic cell
2+solution, with graphite or noble metal, make electrode, switch on power and the periodic variation sense of current, after electrolysis a period of time, just can in the bottom of electrolytic cell, collect nickel powder with magnetic material like this, the pattern of nickel powder and large I are controlled by changing electrolytic condition, this method is more ancient, although be applied industrial, too high owing to consuming, its development is restricted.(3) hydrogen reduction method, this method is simple to operate, and cost is lower, is convenient in industrial popularization, but must uses high-tension apparatus and catalyst, and be difficult to obtain the nickel powder that particle diameter is less.Consider and produce simple, lower-cost production in enormous quantities supply and demand, research has occurred that liquid phase reduction, the method are that the mixture of nickel precursor, organic solution and reducing agent is heated to 50 ~ 450 ℃ of reactions, obtain nano particle.But in the organic solvent in this method, comprise a lot of ethers, saturated hydrocarbons, unsaturated hydro carbons and some organic acids, produced a large amount of poisonous byproducts, very large to ambient influnence.Therefore, seek that a kind of production technology is simple, production cost just seems very important compared with preparation method low, that environmental pollution is few, nickel nanocrystal is thin.
Summary of the invention
The object of the present invention is to provide the nanocrystalline environment-friendly preparation method thereof of a kind of nickel, it is simple that it has production technology, and production cost is lower, the advantage that environmental pollution is few, and the nickel nanocrystal of preparation evenly, purity is high, single disperses, and average grain diameter is not more than the nickel nanocrystal of 20nm.
The present invention is achieved like this, and described preparation method comprises the following steps: 1) four water nickel acetates, sodium borohydride, Choline Chloride and urea are mixed according to the ratio of mass ratio 2:1:6:6, fully grind stand-by; 2) above-mentioned mixture is put in the reactor cleaning up and is heated to 140 ~ 160 ℃, and be incubated 4 ~ 6h; 3) above-mentioned reacted mixture cleaned, filter, can obtain high-purity, more even, monodispersed nickel nanocrystal after dry.The quality of described four water nickel acetates, sodium borohydride, Choline Chloride and urea is respectively 1.0g, 0.5g, 3.0g and 3.0g.In described reactor, heating-up temperature is 140 ℃, 150 ℃ and 160 ℃.Described temperature retention time is 4 h, 5h and 6h.
Technique effect of the present invention is: the invention has the advantages that the environment-friendly preparation method thereof that a kind of nickel is nanocrystalline, with free of contamination sodium borohydride as reducing agent, with the urea that can recycle completely and Choline Chloride as fused-salt medium, and step is very simple, the nano nickel crystal grain purity prepared is high, uniform particles, good dispersion, and average grain diameter is within 10 ~ 20nm.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the embodiment of the present invention 3 products obtained therefroms.
Fig. 2 is the high power Electronic Speculum figure of the embodiment of the present invention 3 products obtained therefroms.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail;
Embodiment 1
The environment-friendly preparation method thereof that nickel is nanocrystalline, takes 1.0g tetra-water nickel acetates, 0.5g sodium borohydride, 3.0g Choline Chloride, 3.0g urea; After they are put in agate mortar and are fully ground, be transferred in the reactor of 50ml, be then heated to 140 ℃ of insulation 4h; Then the reactant in reactor is taken out and clean, filter, be dried, just can obtain nickel nanocrystal.After XRD and SEM characterize, this nickel nanocrystal purity is very high, uniform particles, do not find bonded particulate, and average grain diameter is in 15nm left and right.
Embodiment 2
The environment-friendly preparation method thereof that nickel is nanocrystalline, takes 2g tetra-water nickel acetates, 1g sodium borohydride, 6g Choline Chloride, 6.0g urea; After they are put in agate mortar and are fully ground, be transferred in the reactor of 100ml, be then heated to 150 ℃ of insulation 5h; Then the reactant in reactor is taken out and clean, filter, be dried, just can obtain nickel nanocrystal.After XRD and SEM characterize, this nickel nanocrystal purity is very high, uniform particles, do not find bonded particulate, and average grain diameter is in 16nm left and right.
Embodiment 3
The environment-friendly preparation method thereof that nickel is nanocrystalline, takes 1.0g tetra-water nickel acetates, 0.5g sodium borohydride, 3.0g Choline Chloride, 3.0g urea; After they are put in agate mortar and are fully ground, be transferred in the reactor of 50ml, be then heated to 160 ℃ of insulation 6h; Then the reactant in reactor is taken out and clean, filter, be dried, just can obtain nickel nanocrystal.After XRD and SEM characterize, this nickel nanocrystal purity is very high, uniform particles, do not find bonded particulate, and average grain diameter is in 17nm left and right.As shown in Figure 1, high power Electronic Speculum figure as shown in Figure 2 for the XRD figure of products obtained therefrom.
Claims (4)
1. the nanocrystalline environment-friendly preparation method thereof of nickel, is characterized in that, described preparation method comprises the following steps:
1) four water nickel acetates, sodium borohydride, Choline Chloride and urea are mixed according to the ratio of mass ratio 2:1:6:6, fully grind stand-by;
2) above-mentioned mixture is put in the reactor cleaning up and is heated to 140 ~ 160 ℃, and be incubated 4 ~ 6h;
3) above-mentioned reacted mixture cleaned, filter, can obtain high-purity, more even, monodispersed nickel nanocrystal after dry.
2. the nanocrystalline environment-friendly preparation method thereof of a kind of nickel as claimed in claim 1, is characterized in that, the quality of described four water nickel acetates, sodium borohydride, Choline Chloride and urea is respectively 1.0g, 0.5g, 3.0g and 3.0g.
3. the nanocrystalline environment-friendly preparation method thereof of a kind of nickel as claimed in claim 1, is characterized in that, in described reactor, heating-up temperature is 140 ℃, 150 ℃ and 160 ℃.
4. the nanocrystalline environment-friendly preparation method thereof of a kind of nickel as claimed in claim 1, is characterized in that, described temperature retention time is 4 h, 5h and 6h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105197994A (en) * | 2015-11-05 | 2015-12-30 | 南昌航空大学 | Organic molten salt method for preparation of rod-assembled spherical BiOCl nanoparticles |
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Application publication date: 20140409 |