CN103586482B - The preparation method of nano nickel under a kind of microwave, ultraviolet irradiation - Google Patents
The preparation method of nano nickel under a kind of microwave, ultraviolet irradiation Download PDFInfo
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- CN103586482B CN103586482B CN201310506745.0A CN201310506745A CN103586482B CN 103586482 B CN103586482 B CN 103586482B CN 201310506745 A CN201310506745 A CN 201310506745A CN 103586482 B CN103586482 B CN 103586482B
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Abstract
The present invention relates to the preparation method of nano nickel under a kind of microwave, ultraviolet irradiation, belong to field of nano material preparation. Carry out as steps described below: by 30? min ultrasonic disperse, by organic modifier? (5wt%-20wt%)? it is dissolved in dehydrated alcohol with ethanedioic acid nickel. When reactant mixture is warming up to 60? DEG C time, dropwise dropping NaOH alcoholic solution, regulate reactant liquor pH? is value extremely? 12. Does is then, under microwave, ultraviolet irradiation, dropwise dropping 0.04-0.5mol/L hydrazine hydrate alcoholic solution, under magnetic stirring, warming up to 80-100 DEG C, reacts 30-120? min, is prepared for various sizes of nano nickle granules. The nano nickle granules of preparation is cooled to room temperature and is stored in ethanol solution. The nano nickel prepared by the method, grain diameter is little, even size distribution, good dispersion, and the method reaction condition is easily controllable, low cost, the advantage of processing technology and simple flow.
Description
Technical field
The present invention relates to the preparation method of nano nickel under a kind of microwave, ultraviolet irradiation, belong to field of nano material preparation.
Background technology
Nano metal has, in catalysis, photochemistry, magnetic, conduction, biology etc., the physicochemical characteristics being different from reguline metal material, and the pattern of nano-metal particle directly influences these character. Morphology control synthesis and the applied research of nano metal belong to the important directions in investigation of materials field, utilizing surfactant to participate in chemosynthesis, the preparation and the applied research that carry out the nano metal of particle size and morphology control have far-reaching theory and using value. With the slaine of nickel for parent, in aqueous solution or organic solution, utilize the organic modifier (such as many carboxyls, polyhydroxy Organic substance etc.) with different functional groups, at different preparation conditions, carry out the study on the synthesis of the nano nickel of particle size and morphology control. Nano nickel morphology control study on the synthesis discloses the formation of nano metal crystal face and the relation of preparation condition, and the morphology control synthesis of nano metal is had directive significance.
At present, the preparation method having many nano nickle granules, such as wet-chemical reducing process, microemulsion method and hydrothermal synthesis method. In order to avoid the oxidation of nano nickle granules, reaction is made to carry out under organic solvent medium, as: oxolane, six decyl amine, ethylene glycol and ethanol, it is possible to prepare the nano nickle granules of pure phase. Compared with other organic solvent, ethanol is a kind of being easy to get and green solvent. Additionally, generally select organic modifier, as: sodium carboxymethyl cellulose, sulfonated cis-butadiene rubber, cetyl trimethylammonium bromide, tetraethylammonium bromide and tetrabutyl ammonium bromide, control the size of nano-particle, pattern, inductive formation different size, pattern nano nickle granules. At present, utilizing microwave, the penetrance of ultraviolet irradiation, selection heating property is heat source for reaction, selects the synthesis of highly concentrated nano metal that suitable organic modifier carries out pattern, size Control just becoming the new direction of nano material synthesis.
When low-temp reaction, utilizing microwave, ultraviolet irradiation, we have prepared the ball shaped nano nickel granule that mean diameter is 8-287nm, distribution of sizes is 5-363nm, dispersive property is good. The method reaction condition is easily controllable, low cost, the advantage of processing technology and simple flow.
Summary of the invention
The present invention proposes a kind of by adding the template as control nano nickel size of the organic modifier containing different functional groups, at different microwaves, under the ultraviolet irradiation time, by changing reaction condition parameter, the method preparing different-grain diameter nano nickel.
Its preparation method is as follows:
By 30min ultrasonic disperse, organic modifier (5wt%-20wt%) and ethanedioic acid nickel are dissolved in dehydrated alcohol. When reactant mixture is warming up to 60 DEG C, dropwise drip NaOH (1.0M, 20mL) alcoholic solution, regulate reacting liquid pH value to 12. Then, under microwave, ultraviolet irradiation, (microwave power is 500w; Ultraviolet wavelength is 254nm, and power is 500w), dropwise dropping 0.04-0.5mol/L hydrazine hydrate alcoholic solution, under magnetic stirring, is warming up to 80-100 DEG C, reacts 30-120min. The nano nickle granules of preparation is cooled to room temperature and is stored in ethanol solution.
The above-mentioned organic modifier containing different functional groups refers to double; two (p-sulfonyl-phenyl) the Phenylphosphine di-potassium of two hydrations, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane or polyoxyethylene.
Wherein the ratio of organic modifier, ethanedioic acid nickel and dehydrated alcohol is (0.006-0.12): (0.12-0.6): 70 (g/g/mL).
Above-mentioned ethanedioic acid nickel and the ratio of hydrazine hydrate alcoholic solution are (0.12-0.6): 10g/mL.
The nano nickel prepared by the method, grain diameter is little, even size distribution, good dispersion, and the method reaction condition is easily controllable, low cost, the advantage of processing technology and simple flow.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1
Weigh the ethanedioic acid nickel of double; two (p-sulfonyl-phenyl) the Phenylphosphine di-potassium of 0.015g bis-hydration and 0.3g, under 30min ultrasonic wave added so that it is be dissolved in 70mL dehydrated alcohol, be then transferred in the three-neck flask of 250mL. Solution temperature is risen to 60 DEG C, dropwise drips NaOH (1.0M, 20mL) alcoholic solution, regulate reacting liquid pH value to 12. Under microwave exposure and stirring, dropwise dropping hydrazine hydrate alcoholic solution (0.1M, 10mL), is warming up to 80 DEG C, reacts 30min. After reaction terminates, obtain average diameter to be 36nm, distribution of sizes be the nano nickle granules of 8 59nm.
Embodiment 2
Weigh the ethanedioic acid nickel of double; two (p-sulfonyl-phenyl) the Phenylphosphine di-potassium of 0.07g bis-hydration and 0.45g, under 30min ultrasonic wave added so that it is be dissolved in 70mL dehydrated alcohol, be then transferred in the three-neck flask of 250mL. Solution temperature is risen to 60 DEG C, dropwise drips NaOH (1.0M, 20mL) alcoholic solution, regulate reacting liquid pH value to 12. Under microwave exposure and stirring, dropwise dropping hydrazine hydrate alcoholic solution (0.35M, 10mL), is warming up to 80 DEG C, reacts 120min. After reaction terminates, obtain average diameter to be 8nm, distribution of sizes be the nano nickle granules of 5 41nm.
Embodiment 3
Weigh the ethanedioic acid nickel of double; two (p-sulfonyl-phenyl) the Phenylphosphine di-potassium of 0.05g bis-hydration and 0.5g, under 30min ultrasonic wave added so that it is be dissolved in 70mL dehydrated alcohol, be then transferred in the three-neck flask of 250mL. Solution temperature is risen to 60 DEG C, dropwise drips NaOH (1.0M, 20mL) alcoholic solution, regulate reacting liquid pH value to 12. Under microwave exposure and stirring, dropwise dropping hydrazine hydrate alcoholic solution (0.25M, 10mL), is warming up to 80 DEG C, reacts 60min. After reaction terminates, obtain average diameter to be 87nm, distribution of sizes be the nano nickle granules of 45 103nm.
Embodiment 4
Weigh the ethanedioic acid nickel of double; two (p-sulfonyl-phenyl) the Phenylphosphine di-potassium of 0.03g bis-hydration and 0.2g, under 30min ultrasonic wave added so that it is be dissolved in 70mL dehydrated alcohol, be then transferred in the three-neck flask of 250mL. Solution temperature is risen to 60 DEG C, dropwise drips NaOH (1.0M, 20mL) alcoholic solution, regulate reacting liquid pH value to 12. Under microwave exposure and stirring, dropwise dropping hydrazine hydrate alcoholic solution (0.07M, 10mL), is warming up to 80 DEG C, reacts 90min. After reaction terminates, obtain average diameter to be 19nm, distribution of sizes be the nano nickle granules of 7 46nm.
Embodiment 5
Weigh the ethanedioic acid nickel of 0.06g polyoxyethylene and 0.6g, under 30min ultrasonic wave added so that it is be dissolved in 70mL dehydrated alcohol, be then transferred in the three-neck flask of 250mL. Solution temperature is risen to 60 DEG C, dropwise drips NaOH (1.0M, 20mL) alcoholic solution, regulate reacting liquid pH value to 12. Under microwave exposure and stirring, dropwise dropping hydrazine hydrate alcoholic solution (0.5M, 10mL), is warming up to 100 DEG C, reacts 120min. After reaction terminates, obtain average diameter to be 69nm, distribution of sizes be the nano nickle granules of 29 101nm.
Embodiment 6
Weigh the ethanedioic acid nickel of 0.12g γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and 0.15g, under 30min ultrasonic wave added so that it is be dissolved in 70mL dehydrated alcohol, be then transferred in the three-neck flask of 250mL. Solution temperature is risen to 60 DEG C, dropwise drips NaOH (1.0M, 20mL) alcoholic solution, regulate reacting liquid pH value to 12. Under microwave exposure and stirring, dropwise dropping hydrazine hydrate alcoholic solution (0.05M, 10mL), is warming up to 100 DEG C, reacts 90min. After reaction terminates, obtain average diameter to be 43nm, distribution of sizes be the nano nickle granules of 22 84nm.
Embodiment 7
Weigh γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane of 0.016g and the ethanedioic acid nickel of 0.32g, under 30min ultrasonic wave added so that it is be dissolved in 70mL dehydrated alcohol, be then transferred in the three-neck flask of 250mL. Solution temperature is risen to 60 DEG C, dropwise drips NaOH (1.0M, 20mL) alcoholic solution, regulate reacting liquid pH value to 12. Under microwave exposure and stirring, dropwise dropping hydrazine hydrate alcoholic solution (0.15M, 10mL), is warming up to 90 DEG C, reacts 60min. After reaction terminates, obtain average diameter to be 287nm, distribution of sizes be the nano nickle granules of 82 363nm.
Embodiment 8
Weigh the ethanedioic acid nickel of 0.006g polyoxyethylene and 0.12g, under 30min ultrasonic wave added so that it is be dissolved in 70mL dehydrated alcohol, be then transferred in the three-neck flask of 250mL. Solution temperature is risen to 60 DEG C, dropwise drips NaOH (1.0M, 20mL) alcoholic solution, regulate reacting liquid pH value to 12. Under microwave exposure and stirring, dropwise dropping hydrazine hydrate alcoholic solution (0.04M, 10mL), is warming up to 90 DEG C, reacts 30min. After reaction terminates, obtain average diameter to be 72nm, distribution of sizes be the nano nickle granules of 32 133nm.
Claims (3)
1. the preparation method of nano nickel under a microwave, ultraviolet irradiation, it is characterised in that preparation method is as follows:
By 30min ultrasonic disperse, the organic modifier of 5wt%-20wt% and ethanedioic acid nickel are dissolved in dehydrated alcohol; When reactant mixture is warming up to 60 DEG C, dropwise drip the NaOH alcoholic solution of 1.0M, 20mL, regulate reacting liquid pH value to 12; Then, it is 500w at microwave power; Ultraviolet wavelength is 254nm, and power is under the microwave of 500w, ultraviolet irradiation, and dropwise dropping 0.04-0.5mol/L hydrazine hydrate alcoholic solution, under magnetic stirring, is warming up to 80-100 DEG C, reacts 30-120min; The nano nickle granules of preparation is cooled to room temperature and is stored in ethanol solution;
Selected organic modifier refers to double; two (p-sulfonyl-phenyl) the Phenylphosphine di-potassium of two hydrations, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane or polyoxyethylene.
2. microwave according to claim 1, the preparation method of nano nickel under ultraviolet irradiation, it is characterised in that wherein organic modifier, ethanedioic acid nickel and dehydrated alcohol ratio be (0.006-0.12): (0.12-0.6): 70 (g/g/mL).
3. microwave according to claim 1, the preparation method of nano nickel under ultraviolet irradiation, it is characterised in that wherein the ratio of ethanedioic acid nickel and hydrazine hydrate alcoholic solution is (0.12-0.6): 10g/mL.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101007357A (en) * | 2007-01-22 | 2007-08-01 | 中山大学 | Nanometer nickel powder and its preparation method |
| CN101147978A (en) * | 2007-10-17 | 2008-03-26 | 江苏大学 | Microwave auxiliary liquid phase reduction method preparing needle-shaped nanometer nickel |
| CN101791704A (en) * | 2010-03-25 | 2010-08-04 | 江苏大学 | Method for preparing nano silver |
| CN102179527A (en) * | 2011-05-10 | 2011-09-14 | 湖南省娄底维亚科技有限公司 | Method for preparing nano nickel powder |
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| JP2006336060A (en) * | 2005-06-01 | 2006-12-14 | Sumitomo Metal Mining Co Ltd | Nickel particle powder and production method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101007357A (en) * | 2007-01-22 | 2007-08-01 | 中山大学 | Nanometer nickel powder and its preparation method |
| CN101147978A (en) * | 2007-10-17 | 2008-03-26 | 江苏大学 | Microwave auxiliary liquid phase reduction method preparing needle-shaped nanometer nickel |
| CN101791704A (en) * | 2010-03-25 | 2010-08-04 | 江苏大学 | Method for preparing nano silver |
| CN102179527A (en) * | 2011-05-10 | 2011-09-14 | 湖南省娄底维亚科技有限公司 | Method for preparing nano nickel powder |
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