CN103785826B - A kind of preparation method of modified Nano nickel powder - Google Patents
A kind of preparation method of modified Nano nickel powder Download PDFInfo
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- CN103785826B CN103785826B CN201410057099.9A CN201410057099A CN103785826B CN 103785826 B CN103785826 B CN 103785826B CN 201410057099 A CN201410057099 A CN 201410057099A CN 103785826 B CN103785826 B CN 103785826B
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Abstract
The invention discloses a kind of preparation method of modified Nano nickel powder.The method with mercaptan, silane coupler, cationic surfactant, corrosion inhibiter and organic solvent containing sulfydryl for raw material, surface modification is carried out to nano-nickel powder, prepare modified Nano nickel powder, solve nano-nickel powder easily reunite, oxidizable, with the problem of other materials compound tense intermiscibility difference.The method production technology is simple, and equipment investment is little, and energy consumption is low, non-environmental-pollution, and modified Nano nickel powder applied range, is conducive to applying, has broad 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 to the material having at least one dimension to be in nanoscale scope (1-100nm) or to be made up of as elementary cell them in three dimensions.Because the structure of nano material is different from conventional material, the surface atom of nano material sharply increases along with the reduction of particle diameter with the ratio of total atom number, thus demonstrate strong bulk effect (i.e. small-size effect), quantum size effect, skin effect and macro quanta tunnel effect, nano material is made to have property in optical, electrical, magnetic, thermodynamics and chemical reaction etc., 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 act as very important role in modern industry, national defence and high technology 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, optical switch material, sensing 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 the stuctures and properties difference of nano metal material and conventional metal material is large, therefore, nano metal material exist easily reunite, oxidizable, with the problem of other materials compound tense intermiscibility difference, this will make nano metal material proper property can not obtain fully or completely playing.For making nano metal material stable performance, method the most simple carries out surface modification to nano metal material exactly, stop nano metal material particle growth and reunion, improve the dispersion stabilization of nano metal material, can give nano metal material new function simultaneously.
Nano-nickel powder is the same with other nano metal material, same existence is easily reunited, oxidizable, with the problem of other materials compound tense intermiscibility difference, the present invention with mercaptan, silane coupler, cationic surfactant, corrosion inhibiter and organic solvent containing sulfydryl for raw material, surface modification is carried out to nano-nickel powder, prepare modified Nano nickel powder, solve nano-nickel powder easily reunite, oxidizable, with the problem of other materials compound tense intermiscibility difference, there is important practical significance.At present, home and abroad is about using mercaptan simultaneously, containing the silane coupler of sulfydryl and the research of corrosion inhibiter modified Nano nickel powder and the rarely seen report of technology.
Summary of the invention
The preparation method of a kind of modified Nano nickel powder of the present invention, there is provided a kind of with mercaptan, silane coupler, cationic surfactant, corrosion inhibiter and organic solvent containing sulfydryl for raw material, surface modification is carried out to nano-nickel powder, prepare the method for modified Nano nickel powder, solve nano-nickel powder easily reunite, oxidizable, with the problem of other materials compound tense intermiscibility difference, 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 applying, 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, after stirring 0.1h ~ 5.0h, add nano-nickel powder again, be 20kHz ~ 1MHz in frequency further, power is under the ultrasonic wave peptizaiton of 30W ~ 15kW, stirring reaction 0.1h ~ 20.0h, then successively through centrifugation, absolute ethanol washing, centrifugation, deionized water is washed, centrifugation, vacuum drying, grinding and 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, forms corresponding mercaptan nickel respectively on nano-nickel powder surface; But it is stable alkyl hydrosulfide nickel that mercaptan and nano-nickel powder react the mercaptan nickel formed, and can not be hydrolyzed, what stay on nano-nickel powder surface is nonpolar group; And react the trimethoxy silica-based propanethiol nickel or the silica-based propanethiol nickel of triethoxy that the mercaptan nickel formed is instability, the silica-based [-Si (OCH of trimethoxy wherein containing silane coupler and the nano-nickel powder of sulfydryl
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 and the silane coupler modified nano-nickel powder containing sulfydryl simultaneously, by changing the mass percent of mercaptan and the silane coupler containing sulfydryl in formula, with regulate and control mercaptan and containing the silane coupler of sulfydryl at the mass ratio of nano-nickel powder surface reaction, the amount of modified Nano nickel powder surface polar groups and non-polar group is made to realize controllable adjustment, thus the hydrophily of regulation and control modified Nano nickel powder and lipophile, this is conducive to the dispersibility in different system improving modified Nano nickel powder, with the demand of satisfied different industrial circle.
The preparation method of a kind of modified Nano nickel powder of the present invention, two of its outstanding feature is: during modified Nano nickel powder, employ corrosion inhibiter simultaneously, can, at nano-nickel powder adsorption corrosion inhibiter, be conducive to improving 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, iso-butyl mercaptan, butyl mercaptan, tertiary butyl mercaptan, isoamyl mercaptan, n-amylmercaptane, n-hexyl mercaptan, n octylmercaptan, 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 benzyl dimethyl 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 dodecyldimethylamine yl pyridines ammonium chloride and dodecyldimethylamine yl pyridines 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.
Detailed description of the invention
Here is the non-limiting example of the preparation method of a kind of modified Nano nickel powder of the present invention.The providing of these examples is only used to the object illustrated, can not be interpreted as limitation of the invention.Because without departing from the spirit and scope of the present invention, many conversion can be carried out 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, after stirring 0.2h, add nano-nickel powder again, be 25kHz in frequency further, power is under the ultrasonic wave peptizaiton of 10kW, stir 2.0h, then successively through centrifugation, absolute ethanol washing, centrifugation, deionized water is washed, centrifugation, vacuum drying, grinding and technical process of sieving, prepare modified Nano nickel powder.
Embodiment 2
According to above-mentioned mass percent, successively by butyl mercaptan, phenethyl mercaptan, 3-mercaptopropyl trimethoxysilane, DTAB, dodecyldimethylamine yl pyridines 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, after stirring 0.2h, add nano-nickel powder again, be 28kHz in frequency further, power is under the ultrasonic wave peptizaiton of 6.5kW, stir 3.0h, then successively through centrifugation, absolute ethanol washing, centrifugation, deionized water is washed, centrifugation, vacuum drying, grinding and technical process of sieving, prepare modified Nano nickel powder.
Embodiment 3
According to above-mentioned mass percent, successively by n-dodecyl mercaptan, n-amylmercaptane, 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, after stirring 0.7h, add nano-nickel powder again, be 60kHz in frequency further, power is under the ultrasonic wave peptizaiton of 8kW, stir 3.0h, then successively through centrifugation, absolute ethanol washing, centrifugation, deionized water is washed, centrifugation, vacuum drying, grinding and technical process of sieving, prepare modified Nano nickel powder.
Embodiment 4
According to above-mentioned mass percent, successively by n octylmercaptan, 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, after stirring 0.6h, add nano-nickel powder again, be 60kHz in frequency further, power is under the ultrasonic wave peptizaiton of 2kW, stir 6.5h, then successively through centrifugation, absolute ethanol washing, centrifugation, deionized water is washed, centrifugation, vacuum drying, grinding and technical process of sieving, prepare modified Nano nickel powder.
Embodiment 5
According to above-mentioned mass percent, successively by hexadecyl mercaptan, benzyl mercaptan, 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, after stirring 0.5h, add nano-nickel powder again, be 28kHz in frequency further, power is under the ultrasonic wave peptizaiton of 3.5kW, stir 6.0h, then successively through centrifugation, absolute ethanol washing, centrifugation, deionized water is washed, centrifugation, vacuum drying, grinding and technical process of sieving, prepare modified Nano nickel powder.
Embodiment 6
According to above-mentioned mass percent, successively by tertiary lauryl mercaptan, n-amylmercaptane, 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, after stirring 0.5h, add nano-nickel powder again, be 40kHz in frequency further, power is under the ultrasonic wave peptizaiton of 4kW, stir 4.5h, then successively through centrifugation, absolute ethanol washing, centrifugation, deionized water is washed, centrifugation, vacuum drying, grinding and technical process of sieving, prepare modified Nano nickel powder.
Embodiment 7
According to above-mentioned mass percent, successively by n octylmercaptan, n-dodecyl mercaptan, hexadecyl mercaptan, 3-mercaptopropyltriethoxysilane, 3-mercaptopropyl trimethoxysilane, OTAC, myristyl benzyl dimethyl ammonium chloride, dodecyldimethylamine yl pyridines 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, after stirring 0.3h, add nano-nickel powder again, be 68kHz in frequency further, power is under the ultrasonic wave peptizaiton of 3.5kW, stir 5.0h, then successively through centrifugation, absolute ethanol washing, centrifugation, deionized water is washed, centrifugation, vacuum drying, grinding and 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 octylmercaptan, butyl mercaptan, 3-mercaptopropyltriethoxysilane, 3-mercaptopropyl trimethoxysilane, softex kw ammonium, tetradecyl dimethyl benzyl ammonium, trimethyl chlorination, 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, after stirring 0.2h, add nano-nickel powder again, be 48kHz in frequency further, power is under the ultrasonic wave peptizaiton of 1.5kW, stir 2.5h, then successively through centrifugation, absolute ethanol washing, centrifugation, deionized water is washed, centrifugation, vacuum drying, grinding and technical process of sieving, prepare modified Nano nickel powder.
Claims (6)
1. a preparation method for modified Nano nickel powder, is characterized in that:
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, after stirring 0.1h ~ 5.0h, add nano-nickel powder again, be 20kHz ~ 1MHz in frequency further, power is under the ultrasonic wave peptizaiton of 30W ~ 15kW, stirring reaction 0.1h ~ 20.0h, then successively through centrifugation, absolute ethanol washing, centrifugation, deionized water is washed, centrifugation, vacuum drying, grinding and technical process of sieving, prepare modified Nano nickel powder.
2. 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, iso-butyl mercaptan, butyl mercaptan, tertiary butyl mercaptan, isoamyl mercaptan, n-amylmercaptane, n-hexyl mercaptan, n octylmercaptan, n-nonyl mercaptan, n-dodecyl mercaptan, tertiary lauryl mercaptan, tetradecyl mercaptan, hexadecyl mercaptan, Stearyl mercaptan, benzyl mercaptan and phenethyl mercaptan.
3. preparation method as claimed in claim 1, is characterized in that the silane coupler containing sulfydryl reacting used is any one or two kinds of in 3-mercaptopropyltriethoxysilane and 3-mercaptopropyl trimethoxysilane.
4. 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 benzyl dimethyl 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 dodecyldimethylamine yl pyridines ammonium chloride and dodecyldimethylamine yl pyridines ammonium bromide.
5. 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.
6. 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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CN104985175B (en) * | 2015-07-02 | 2017-03-08 | 广东光华科技股份有限公司 | A kind of method for removing nano metal powder surface anion |
CN105642903B (en) * | 2016-03-01 | 2017-12-22 | 河海大学 | The process for dispersing that a kind of nickel nanowire surface non-covalent modification is modified |
CN105798287B (en) * | 2016-04-29 | 2017-12-22 | 河海大学 | The process for dispersing that a kind of nickel nanowire surface covalent modification is modified |
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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