CN103785826A - Method for preparing modified nanometer nickel powder - Google Patents
Method for preparing modified nanometer nickel powder Download PDFInfo
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- CN103785826A CN103785826A CN201410057099.9A CN201410057099A CN103785826A CN 103785826 A CN103785826 A CN 103785826A CN 201410057099 A CN201410057099 A CN 201410057099A CN 103785826 A CN103785826 A CN 103785826A
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Abstract
The invention discloses a method for preparing modified nanometer nickel powder. According to the method, sulfur alcohol, a silane coupling agent with sulfydryl, a cationic surface active agent, a corrosion inhibitor and organic solvent are used as raw materials, surface modification is conducted on the nanometer nickel powder, and then the modified nanometer nickel powder is obtained through preparation. The problems that the nanometer nickel powder is prone to agglomeration and oxidization, and intermiscibility is poor when the nanometer nickel powder and other materials are composited are solved. The method is simple and feasible in production process, small in investment on equipment, low in energy consumption, and free of environment pollution, and the modified nanometer nickel powder is wide in application range, and capable of being popularized and applied, and has wide application prospects.
Description
Technical field
The present invention relates to a kind of preparation method of modified Nano nickel powder, belong to nano metal material field.
Background technology
Nano material refers in three dimensions, to have one dimension at least in nanoscale scope (1-100nm) or the material that is made up of as elementary cell them.Because the structure of nano material is different from conventional material, the surface atom of nano material sharply increases along with reducing of particle diameter with the ratio of total atom number, thereby demonstrate strong bulk effect (being small-size effect), quantum size effect, skin effect and macro quanta tunnel effect, make nano material there is property at aspects such as optical, electrical, magnetic, thermodynamics and chemical reactions, be a kind of important functional material, have broad application prospects.In recent years, nano material receives much concern, and nano material has become the study hotspot of material science.
As an aspect of nano material, metal nano material and alloy nano-material are serving as very important role in modern industry, national defence and high-tech development, have broad application prospects.Nano metal material can be widely used in the fields such as nano ceramic material, nano magnetic material, rocket combustion-supporting, nano catalytic material, nanometer medical material, nano-textile material, nano environmental protection material, optical communication material, electromagnetic wave absorption material, electromagnetic functional material, nanometer conductive material, nonlinear optical material, photoswitch material, sensor element material, structural material, nano composite material, micropore gas diffusion barrier, computer, household electrical appliance and engineering material.
Because nano metal material belongs to metastable material, responsive especially to environmental factors such as temperature, vibration, illumination, magnetic field and atmosphere, likely grow up voluntarily at normal temperatures, because structure and the performance difference of nano metal material and common metal material are large, therefore, nano metal material exist easily reunite, oxidizable, poor with other materials compound tense intermiscibility problem, this will make nano metal material proper property can not obtain fully or performance completely.For making nano metal material stable performance, the most simple method is carried out surface modification to nano metal material exactly, stop nano metal material particle grow up and reunite, improve the dispersion stabilization of nano metal material, can give the function that nano metal material is new simultaneously.
Nano-nickel powder is the same with other nano metal material, same exist easily reunite, oxidizable, poor with other materials compound tense intermiscibility problem, the present invention take mercaptan, containing silane coupler, cationic surfactant, corrosion inhibiter and the organic solvent of sulfydryl as raw material, nano-nickel powder is carried out to surface modification, prepare modified Nano nickel powder, solve nano-nickel powder easily reunite, oxidizable, with the poor problem of other materials compound tense intermiscibility, there is important practical significance.At present, home and abroad is about use mercaptan, contain the silane coupler of sulfydryl and the research of corrosion inhibiter modified Nano nickel powder and the rarely seen report of technology simultaneously.
Summary of the invention
The preparation method of a kind of modified Nano nickel powder of the present invention, provide a kind of take mercaptan, containing silane coupler, cationic surfactant, corrosion inhibiter and the organic solvent of sulfydryl as raw material, nano-nickel powder is carried out to surface modification, prepare the method for modified Nano nickel powder, solve nano-nickel powder easily reunite, oxidizable, with the poor problem of other materials compound tense intermiscibility, the method production technology is simple, equipment investment is little, energy consumption is low, non-environmental-pollution, modified Nano nickel powder applied range, is conducive to apply, and has broad application prospects.
The preparation method of a kind of modified Nano nickel powder of the present invention, adopts following technical scheme:
According to mercaptan, containing the silane coupler of sulfydryl, cationic surfactant, corrosion inhibiter, the mass percent of organic solvent and nano-nickel powder is (0.001%～50%): (0.00001%～50%): (0.001%～40%): (0.001%～25%): (0.001%～98%): the ratio of (0.001%～75%), successively by mercaptan, containing the silane coupler of sulfydryl, cationic surfactant and corrosion inhibiter add in organic solvent, be 20kHz～1MHz in frequency, power is under the ultrasonic wave peptizaiton of 30W～15kW, stir after 0.1h～5.0h, add again nano-nickel powder, be further 20kHz～1MHz in frequency, power is under the ultrasonic wave peptizaiton of 30W～15kW, stirring reaction 0.1h～20.0h, then pass through successively centrifugation, absolute ethanol washing, centrifugation, deionized water washing, centrifugation, vacuum drying, grind and the technical process of sieving, prepare modified Nano nickel powder.
The preparation method of a kind of modified Nano nickel powder of the present invention, one of its outstanding feature is: all contain sulfydryl due to mercaptan with containing the silane coupler of sulfydryl, all can react with nano-nickel powder, form corresponding mercaptan nickel respectively on nano-nickel powder surface; But mercaptan reacts the mercaptan nickel forming with nano-nickel powder be stable alkyl hydrosulfide nickel, can not be hydrolyzed, and what stay on nano-nickel powder surface is nonpolar group; The silica-based propanethiol nickel of unsettled trimethoxy or the silica-based propanethiol nickel of triethoxy and react containing the silane coupler of sulfydryl the mercaptan nickel forming with nano-nickel powder, the silica-based [Si (OCH of trimethoxy wherein
3)
3] or the silica-based [Si (OCH of triethoxy
2cH
3)
3] be easily hydrolyzed to the silica-based [Si (OH) of trihydroxy of polarity
3] group ,-Si (OH)
3between group, mutually condensation forms the SiOSi key of polarity again, and what stay on nano-nickel powder surface is the group of polarity; Therefore, when using mercaptan simultaneously and containing the silane coupler modified nano-nickel powder of sulfydryl, mercaptan and the mass percent containing the silane coupler of sulfydryl in can filling a prescription by change, to regulate and control mercaptan and to contain the silane coupler of sulfydryl at the mass ratio of nano-nickel powder surface reaction, make the amount of modified Nano nickel powder surface polarity group and non-polar group realize controllable adjustment, thereby hydrophily and the lipophile of regulation and control modified Nano nickel powder, this is conducive to improve the dispersibility in different systems of modified Nano nickel powder, to meet the demand of different industrial circles.
The preparation method of a kind of modified Nano nickel powder of the present invention, two of its outstanding feature is: when modified Nano nickel powder, use corrosion inhibiter simultaneously, can, at nano-nickel powder adsorption corrosion inhibiter, be conducive to improve nano-nickel powder heat endurance and oxidation resistent susceptibility.
The preparation method of a kind of modified Nano nickel powder of the present invention, is characterized in that mercaptan used is any one or more in n-pro-pyl mercaptan, isopropyl mercaptan, tert-butyl mercaptan, sec-butyl mercaptan, isobutyl group mercaptan, normal-butyl mercaptan, tertiary butyl mercaptan, isopentyl mercaptan, n-pentyl mercaptan, n-hexyl mercaptan, n-octyl mercaptan, n-nonyl mercaptan, n-dodecyl mercaptan, tertiary lauryl mercaptan, tetradecyl mercaptan, hexadecyl mercaptan, Stearyl mercaptan, benzyl mercaptan and phenethyl mercaptan.
The preparation method of a kind of modified Nano nickel powder of the present invention, is characterized in that the silane coupler containing sulfydryl used is any one or two kinds of in 3-mercaptopropyltriethoxysilane and 3-mercaptopropyl trimethoxysilane.
The preparation method of a kind of modified Nano nickel powder of the present invention, it is characterized in that cationic surfactant used is DTAC, DTAB, dodecyl benzyl dimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium bromide, tetradecyl trimethyl ammonium chloride, TTAB, myristyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium, hexadecyltrimethylammonium chloride, softex kw, cetalkonium chloride, cetyl dimethyl benzyl ammonium bromide, OTAC, Cetyltrimethylammonium bromide, stearyl dimethyl benzyl ammonium chloride, octadecyl dimethyl benzyl ammonium bromide, any one or more in myristyl lutidines ammonium chloride and myristyl lutidines ammonium bromide.
The preparation method of a kind of modified Nano nickel powder of the present invention, is characterized in that corrosion inhibiter used is any one or more in BTA, methyl benzotriazazole, N-hydroxy benzo triazole, 1-hydroxy benzo triazole, 5-carboxy benzotriazole and 4-hydroxy benzo triazole.
The preparation method of a kind of modified Nano nickel powder of the present invention, is characterized in that organic solvent used is any one or more in absolute methanol, absolute ethyl alcohol, isopropyl alcohol, butanols, benzene,toluene,xylene, pentane, hexane, octane, cyclohexane, perchloroethylene, trichloro-ethylene, carrene, chloroform, carbon tetrachloride, carbon disulfide, acetone, butanone, methylisobutylketone, cyclohexanone, methyl acetate, ethyl acetate, propyl acetate, ether, 7 glycol monomethyl ethers, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether and acetonitrile.
The specific embodiment
The preparation method's of a kind of modified Nano nickel powder of the present invention non-limiting example below.The providing of these examples is only used to the object of explanation, can not be interpreted as limitation of the invention.Because without departing from the spirit and scope of the present invention, can carry out many conversion to the present invention.In these embodiments, unless stated otherwise, all percentage all refers to mass percent.
Embodiment 1
According to above-mentioned mass percent, successively by tert-butyl mercaptan, Stearyl mercaptan, 3-mercaptopropyltriethoxysilane, stearyl dimethyl benzyl ammonium chloride, DTAC, 4-hydroxy benzo triazole, BTA, carrene and acetone add in absolute ethyl alcohol, be 25kHz in frequency, power is under the ultrasonic wave peptizaiton of 10kW, stir after 0.2h, add again nano-nickel powder, be further 25kHz in frequency, power is under the ultrasonic wave peptizaiton of 10kW, stir 2.0h, then pass through successively centrifugation, absolute ethanol washing, centrifugation, deionized water washing, centrifugation, vacuum drying, grind and the technical process of sieving, prepare modified Nano nickel powder.
Embodiment 2
According to above-mentioned mass percent, successively by normal-butyl mercaptan, phenethyl mercaptan, 3-mercaptopropyl trimethoxysilane, DTAB, myristyl lutidines ammonium bromide, cetyl dimethyl benzyl ammonium bromide, methyl benzotriazazole, ethylene glycol monoethyl ether, toluene and ethyl acetate add in absolute ethyl alcohol, be 28kHz in frequency, power is under the ultrasonic wave peptizaiton of 6.5kW, stir after 0.2h, add again nano-nickel powder, be further 28kHz in frequency, power is under the ultrasonic wave peptizaiton of 6.5kW, stir 3.0h, then pass through successively centrifugation, absolute ethanol washing, centrifugation, deionized water washing, centrifugation, vacuum drying, grind and the technical process of sieving, prepare modified Nano nickel powder.
Embodiment 3
According to above-mentioned mass percent, successively by n-dodecyl mercaptan, n-pentyl mercaptan, 3-mercaptopropyltriethoxysilane, dodecyl benzyl dimethyl ammonium chloride, Cetyltrimethylammonium bromide, N-hydroxy benzo triazole, BTA, carbon tetrachloride and butanone add in absolute ethyl alcohol, be 60kHz in frequency, power is under the ultrasonic wave peptizaiton of 8kW, stir after 0.7h, add again nano-nickel powder, be further 60kHz in frequency, power is under the ultrasonic wave peptizaiton of 8kW, stir 3.0h, then pass through successively centrifugation, absolute ethanol washing, centrifugation, deionized water washing, centrifugation, vacuum drying, grind and the technical process of sieving, prepare modified Nano nickel powder.
Embodiment 4
According to above-mentioned mass percent, successively by n-octyl mercaptan, tetradecyl mercaptan, 3-mercaptopropyl trimethoxysilane, TTAB, dodecyl dimethyl benzyl ammonium bromide, 1-hydroxy benzo triazole, BTA, dimethylbenzene and isopropyl alcohol add in absolute ethyl alcohol, be 60kHz in frequency, power is under the ultrasonic wave peptizaiton of 2kW, stir after 0.6h, add again nano-nickel powder, be further 60kHz in frequency, power is under the ultrasonic wave peptizaiton of 2kW, stir 6.5h, then pass through successively centrifugation, absolute ethanol washing, centrifugation, deionized water washing, centrifugation, vacuum drying, grind and the technical process of sieving, prepare modified Nano nickel powder.
Embodiment 5
According to above-mentioned mass percent, successively by hexadecyl mercaptan, benzyl mercaptan, normal-butyl mercaptan, 3-mercaptopropyltriethoxysilane, tetradecyl trimethyl ammonium chloride, cetalkonium chloride, 5-carboxy benzotriazole, BTA, cyclohexane chloroform adds in absolute ethyl alcohol, be 28kHz in frequency, power is under the ultrasonic wave peptizaiton of 3.5kW, stir after 0.5h, add again nano-nickel powder, be further 28kHz in frequency, power is under the ultrasonic wave peptizaiton of 3.5kW, stir 6.0h, then pass through successively centrifugation, absolute ethanol washing, centrifugation, deionized water washing, centrifugation, vacuum drying, grind and the technical process of sieving, prepare modified Nano nickel powder.
Embodiment 6
According to above-mentioned mass percent, successively by tertiary lauryl mercaptan, n-pentyl mercaptan, 3-mercaptopropyl trimethoxysilane, octadecyl dimethyl benzyl ammonium bromide, hexadecyltrimethylammonium chloride, BTA, propyl acetate and butanols add in absolute ethyl alcohol, be 40kHz in frequency, power is under the ultrasonic wave peptizaiton of 4kW, stir after 0.5h, add again nano-nickel powder, be further 40kHz in frequency, power is under the ultrasonic wave peptizaiton of 4kW, stir 4.5h, then pass through successively centrifugation, absolute ethanol washing, centrifugation, deionized water washing, centrifugation, vacuum drying, grind and the technical process of sieving, prepare modified Nano nickel powder.
Embodiment 7
According to above-mentioned mass percent, successively by n-octyl mercaptan, n-dodecyl mercaptan, hexadecyl mercaptan, 3-mercaptopropyltriethoxysilane, 3-mercaptopropyl trimethoxysilane, OTAC, myristyl dimethyl benzyl ammonium chloride, myristyl lutidines ammonium chloride, BTA and 4-hydroxy benzo triazole add in absolute ethyl alcohol, be 68kHz in frequency, power is under the ultrasonic wave peptizaiton of 3.5kW, stir after 0.3h, add again nano-nickel powder, be further 68kHz in frequency, power is under the ultrasonic wave peptizaiton of 3.5kW, stir 5.0h, then pass through successively centrifugation, absolute ethanol washing, centrifugation, deionized water washing, centrifugation, vacuum drying, grind and the technical process of sieving, prepare modified Nano nickel powder.
Embodiment 8
The preparation of modified Nano nickel powder:
According to above-mentioned mass percent, successively by Stearyl mercaptan, n-octyl mercaptan, normal-butyl mercaptan, 3-mercaptopropyltriethoxysilane, 3-mercaptopropyl trimethoxysilane, softex kw ammonium, tetradecyl dimethyl benzyl ammonium, the chlorination of dodecyl trimethyl, methyl benzotriazazole, 1-hydroxy benzo triazole, octane, cyclohexanone and methyl acetate add in absolute ethyl alcohol, be 48kHz in frequency, power is under the ultrasonic wave peptizaiton of 1.5kW, stir after 0.2h, add again nano-nickel powder, be further 48kHz in frequency, power is under the ultrasonic wave peptizaiton of 1.5kW, stir 2.5h, then pass through successively centrifugation, absolute ethanol washing, centrifugation, deionized water washing, centrifugation, vacuum drying, grind and the technical process of sieving, prepare modified Nano nickel powder.
Claims (7)
1. a preparation method for modified Nano nickel powder, is characterized in that the technical scheme adopting is:
According to mercaptan, containing the silane coupler of sulfydryl, cationic surfactant, corrosion inhibiter, the mass percent of organic solvent and nano-nickel powder is (0.001%～50%): (0.00001%～50%): (0.001%～40%): (0.001%～25%): (0.001%～98%): the ratio of (0.001%～75%), successively by mercaptan, containing the silane coupler of sulfydryl, cationic surfactant and corrosion inhibiter add in organic solvent, be 20kHz～1MHz in frequency, power is under the ultrasonic wave peptizaiton of 30W～15kW, stir after 0.1h～5.0h, add again nano-nickel powder, be further 20kHz～1MHz in frequency, power is under the ultrasonic wave peptizaiton of 30W～15kW, stirring reaction 0.1h～20.0h, then pass through successively centrifugation, absolute ethanol washing, centrifugation, deionized water washing, centrifugation, vacuum drying, grind and the technical process of sieving, prepare modified Nano nickel powder.
2. preparation method as claimed in claim 1, has following distinguishing feature:
1. all contain sulfydryl due to mercaptan with containing the silane coupler of sulfydryl, all can react with nano-nickel powder, form corresponding mercaptan nickel on nano-nickel powder surface respectively; But mercaptan reacts the mercaptan nickel forming with nano-nickel powder be stable alkyl hydrosulfide nickel, can not be hydrolyzed, and what stay on nano-nickel powder surface is nonpolar group; The silica-based propanethiol nickel of unsettled trimethoxy or the silica-based propanethiol nickel of triethoxy and react containing the silane coupler of sulfydryl the mercaptan nickel forming with nano-nickel powder, the silica-based [Si (OCH of trimethoxy wherein
3)
3] or the silica-based [Si (OCH of triethoxy
2cH
3)
3] be easily hydrolyzed to the silica-based [Si (OH) of trihydroxy of polarity
3] group ,-Si (OH)
3between group, mutually condensation forms the SiOSi key of polarity again, and what stay on nano-nickel powder surface is the group of polarity; Therefore, when using mercaptan simultaneously and containing the silane coupler modified nano-nickel powder of sulfydryl, mercaptan and the mass percent containing the silane coupler of sulfydryl in can filling a prescription by change, to regulate and control mercaptan and to contain the silane coupler of sulfydryl at the mass ratio of nano-nickel powder surface reaction, make the amount of modified Nano nickel powder surface polarity group and non-polar group realize controllable adjustment, thereby hydrophily and the lipophile of regulation and control modified Nano nickel powder, this is conducive to improve the dispersibility in different systems of modified Nano nickel powder, to meet the demand of different industrial circles;
2. when modified Nano nickel powder, use corrosion inhibiter simultaneously, can, at nano-nickel powder adsorption corrosion inhibiter, be conducive to improve nano-nickel powder heat endurance and oxidation resistent susceptibility.
3. preparation method as claimed in claim 1, is characterized in that mercaptan used is any one or more in n-pro-pyl mercaptan, isopropyl mercaptan, tert-butyl mercaptan, sec-butyl mercaptan, isobutyl group mercaptan, normal-butyl mercaptan, tertiary butyl mercaptan, isopentyl mercaptan, n-pentyl mercaptan, n-hexyl mercaptan, n-octyl mercaptan, n-nonyl mercaptan, n-dodecyl mercaptan, tertiary lauryl mercaptan, tetradecyl mercaptan, hexadecyl mercaptan, Stearyl mercaptan, benzyl mercaptan and phenethyl mercaptan.
4. preparation method as claimed in claim 1, is characterized in that the silane coupler containing sulfydryl that reacts used is 3
-any one or two kinds of in mercaptopropyltriethoxysilane and 3-mercaptopropyl trimethoxysilane.
5. preparation method as claimed in claim 1, it is characterized in that cationic surfactant used is DTAC, DTAB, dodecyl benzyl dimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium bromide, tetradecyl trimethyl ammonium chloride, TTAB, myristyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium, hexadecyltrimethylammonium chloride, softex kw, cetalkonium chloride, cetyl dimethyl benzyl ammonium bromide, OTAC, Cetyltrimethylammonium bromide, stearyl dimethyl benzyl ammonium chloride, octadecyl dimethyl benzyl ammonium bromide, any one or more in myristyl lutidines ammonium chloride and myristyl lutidines ammonium bromide.
6. preparation method as claimed in claim 1, is characterized in that corrosion inhibiter used is any one or more in BTA, methyl benzotriazazole, N-hydroxy benzo triazole, 1-hydroxy benzo triazole, 5-carboxy benzotriazole and 4-hydroxy benzo triazole.
7. preparation method as claimed in claim 1, is characterized in that organic solvent used is any one or more in absolute methanol, absolute ethyl alcohol, isopropyl alcohol, butanols, benzene,toluene,xylene, pentane, hexane, octane, cyclohexane, perchloroethylene, trichloro-ethylene, carrene, chloroform, carbon tetrachloride, carbon disulfide, acetone, butanone, methylisobutylketone, cyclohexanone, methyl acetate, ethyl acetate, propyl acetate, ether, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether and acetonitrile.
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| CN105642903A (en) * | 2016-03-01 | 2016-06-08 | 河海大学 | Dispersion method for surface non-covalent modification of nickel nanowire |
| CN105798287A (en) * | 2016-04-29 | 2016-07-27 | 河海大学 | Scattering method for surface covalent modification modification of nickel nanowires |
| CN111732978A (en) * | 2020-06-02 | 2020-10-02 | 上海中太行之光能源有限公司 | Liquid nano combustion material and preparation method thereof |
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