A kind of nickel cluster compound and preparation method thereof
A technology of clusters and methyl groups, applied in the field of nickel clusters and their preparation, to achieve good magnetic properties and strong anisotropy
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[0040] The present invention provides a kind of preparation method of nickel cluster described in above-mentioned technical scheme, comprises the following steps:
[0041] a), Ni(OAc) 4H 2 O, 4-methyl-5-imidazolyl-methanol hydrogen chloride, alkali and solvent are mixed and reacted to obtain a reaction solution;
[0042] b) The reaction solution is crystallized to obtain nickel clusters.
[0043] In the preparation method provided by the invention, first Ni(OAc)·4H 2 O, 4-methyl-5-imidazolyl-methanol hydrogen chloride, base and solvent are mixed for reaction. Wherein, the base is preferably one or more of NaOH, triethylamine, triethanolamine and ethanolamine, more preferably NaOH. The solvent is preferably ethanol or an aqueous ethanol solution. The volume ratio of ethanol to water in the ethanol aqueous solution is preferably 4-6:0.01-2, more preferably 4-5:1-2. The Ni(OAc)·4H 2 O, 4-methyl-5-imidazolyl-methanol hydrogen chloride, the hydroxide group in the alkali and t...
Embodiment 1
[0058] Ni(OAc)·4H 2 O (0.124 g, 0.5 mmol) was dissolved in 25 mL of ethanol. 4-Methyl-5-imidazolyl-methanol hydrogen chloride (0.072g, 0.5mmol) was dissolved in 5mL of ethanol solution, then NaOH (0.020g, 0.5mmol) was added to the alcohol solution, and slowly added to In the solution of the above-mentioned nickel salt, after stirring for 1 hour, filter it, and leave the light green filtrate obtained at room temperature, and after 1 week, a light green massive crystal is obtained, which is the nickel cluster crystal obtained in this example. thing. The yield and purity of the product were analyzed and calculated, and the results were: the yield was about 54%, and the purity of the product was 96%.
[0059] Infrared spectrum analysis is carried out to the above-mentioned light green massive crystal, the result is: IR (KBr, cm -1 ): 3265m, 2913w, 2876w, 2652vw, 2116s, 1626m, 1507m, 1466m, 1438w, 1398vw, 1361vw, 1301vw, 1260m, 1233w, 1168w, 1107w, 1001s, 822m, 782m, vv1, 729w, ...
Embodiment 2
[0070] Ni(OAc)·4H 2 O (0.124g, 0.5mmol) was dissolved in a mixed solution of 25mL ethanol and water (4:1 by volume). 4-Methyl-5-imidazolyl-methanol hydrogen chloride (0.072g, 0.5mmol) was dissolved in 5mL of aqueous solution, then NaOH (0.020g, 0.5mmol) was added to the aqueous solution, and after dissolution, slowly added to the metal salt The solution was stirred for 1 hour and then filtered, and the resulting light green filtrate was placed at room temperature, and after 8 days, light green massive crystals were obtained, which were the nickel clusters prepared in this example. The product and purity of the product were analyzed and calculated, and the results were: the yield was about 43%, and the product purity was 97%.
[0071] Infrared spectrum analysis is carried out to the above-mentioned light green massive crystal that makes, and the result is:
[0072] IR(KBr,cm -1 ): 3269m, 2902w, 2127vs, 1624m, 1504w, 1462m, 1428m, 1258m, 1172vw, 1002s, 831w, 780w, 652vw, 618m...
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