CN104668577B - A kind of nickel micro-and nano-particles and preparation method thereof - Google Patents
A kind of nickel micro-and nano-particles and preparation method thereof Download PDFInfo
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- CN104668577B CN104668577B CN201510060567.2A CN201510060567A CN104668577B CN 104668577 B CN104668577 B CN 104668577B CN 201510060567 A CN201510060567 A CN 201510060567A CN 104668577 B CN104668577 B CN 104668577B
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Abstract
The invention discloses a kind of nickel micro-and nano-particles and preparation method thereof, a certain amount of nickel salt solution is added to containing in sulfaquinoxaline sodium solution in the present invention, product centrifuge separation after reacting, being aged at a certain temperature, leave sediment, the sediment described in deionized water and ethanol washing respectively, ultrasonic disperse, it is dry, corresponding sulfaquinoxaline nickel micro-and nano-particles are made.The present invention, which is successfully realized, prepares metal micro-nano particle to the reaction of different nickel salts and sulfaquinoxaline, obtains the metal-ligand micro-and nano-particles of uniform particle diameter, and have excellent physical and chemical performance.Sulfaquinoxaline nickel micro-and nano-particles have good catalytic activity as catalyst, have broad application prospects in catalytic field.Easy to operate in whole preparation process, cost of material is low, and equipment investment is few, is suitble to mass production.
Description
Technical field
The present invention relates to micro-nano material field, a kind of nickel micro-and nano-particles and preparation method thereof are particularly related to.
Background technique
A kind of emerging science and technology of the nanotechnology as most market application potential, potential importance need not be set
It doubts, some developed countries all put into a large amount of fund and carry out research work.If colonial has set up research in nanotechnology center, Japan
Nanotechnology is classified as one of four big primary study exploration projects of material science at home by portion of culture and education section, many scientific research institutions,
Institution of higher learning also organize scientific research strength, carry out the research work of nanotechnology.
It is to be located at a transitional region at the junction of a cluster of atoms and a macroscopic object that nanoparticle, which is also ultramicro powder, and such system was both
Atypical microscopic system also atypical macrosystem, is a kind of typical Mesoscopic structure, it has skin effect, small size
Effect and macro quanta tunnel effect.When people subdivide macroscopic objects into ultrafine particles (nanoscale), it would indicate that perhaps
Mostly unusual characteristic, the i.e. property of its rare earth nano material optics, calorifics, electricity, magnetics, mechanics and chemical aspect and big
Significant difference will be had when block solid phase ratio, greatly develops new and high technology new product.Therefore nano material for heat-barrier material,
Semiconductor, catalyst etc. have very high development prospect.For the configuration of surface of nano-corpuscule, with partial size
Reduction, surface smooth degree reduces, form scraggly atomic steps, this adds increased the contact surface of chemical reaction,
To improve the effective rate of utilization of catalyst.
For nickel micro Nano material catalyzed coupling reaction, it there is also some problems that needs go to solve.
Firstly, the organic chemist research nickel micro Nano material catalytic performance of profession is specific not enough, to different anti-
The catalytic selectivity of substrate is answered to need to be improved.Whether the factors such as structure and size and pattern for nickel micro Nano material can be right
Catalytic performance impacts, and there is no system in-depth study is carried out, does not more propose how that the design micro-nano catalyst of nickel comes
Improve the efficiency of catalyzed coupling reaction.
Secondly, nickel micro Nano material is compared with palladium catalyst, catalytic activity is not high.Therefore, urging for catalyst is greatly improved
The dosage changed activity, reduce catalyst, and one of the major issue for currently needing to solve.
Summary of the invention
In view of this, preparation process is simple it is an object of the invention to propose that a kind of reaction condition is mild, it is low in cost,
There are nickel micro-and nano-particles of good catalytic and preparation method thereof simultaneously.
Based on above-mentioned purpose nickel micro-and nano-particles provided by the invention and preparation method thereof, specifically includes the following steps:
It weighs sodium sulfaquinoxaline to be dissolved in solvent, obtains sulfaquinoxaline sodium salt solution；
It is soluble in water to weigh nickel salt, obtains nickel salt aqueous solution；
Prepared nickel salt aqueous solution is added in sulfaquinoxaline sodium salt solution, the ultrasonic reaction 12 at 20~80 DEG C
~for 24 hours, wherein initial Ni2+It is 1:0.5~3 with the ratio between the amount of sodium sulfaquinoxaline substance；After reaction, still aging 12~
24h；
By the product centrifuge separation after ageing, sediment is left, respectively the sediment described in deionized water and ethanol washing,
Ultrasonic disperse, it is dry, that is, obtain the sulfaquinoxaline nickel micro-and nano-particles.
Optionally, the sodium sulfaquinoxaline, molecular formula C14H11N4NaO2S, structural formula are as follows:
Optionally, the solvent is one or more of ethyl alcohol, methanol, water.
Optionally, the nickel salt is divalent nickel salt, selected from one of nickel sulfate, nickel chloride, nickel nitrate and nickel acetate or
It is several.
The present invention provides a kind of sulfaquinoxaline nickel micro-and nano-particles and is used as catalyst, and the sulfaquinoxaline nickel is micro-nano
Particle diameter is 300~5000nm, for being catalyzed C-C coupling reaction.
From the above it can be seen that nickel micro-and nano-particles provided by the invention and preparation method thereof, advantage is as follows:
1. compared with palladium salt, the nickel salt cheaper of selection.
2. the nickel micro-and nano-particles are with unique structure and have good catalytic performance, and preparation method is simple.
3. the C-C coupling reaction solvent for use in the present invention is the mixed solution of second alcohol and water, environmentally protective.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of nickel of embodiment of the present invention micro-and nano-particles.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Attached drawing, the present invention is described in more detail.
Embodiment 1
The nickel sulfate solution and 15mmol/L sulfaquinoxaline sodium water solution each 50mL of 5mmol/L are prepared, it is spare；
The aqueous solution mixing of the nickel sulfate solution and 5mL 15mmol/L sodium sulfaquinoxaline of 5mL 5mmol/L is taken respectively,
20 DEG C of stirring ultrasonic reactions for 24 hours, after reaction, still aging 12h.The product centrifuge separation that reaction is obtained, discards clarification
Liquid, the sediment left use deionized water and ethanol washing 3 times respectively, and ultrasonic disperse is dry, i.e. acquisition sulfaquinoxaline nickel
Micro particles.The product is observed with scanning electron microscope (SEM) referring to Fig. 1, and product is granular particle, and size is about 300
~800nm.
Embodiment 2
The nickel nitrate aqueous solution and 10mmol/L sulfaquinoxaline sodium water solution each 50mL of 10mmol/L are prepared, it is spare；
The aqueous solution of the nickel sulfate solution and 5mL 10mmol/L sodium sulfaquinoxaline that take 5mL 10mmol/L respectively is mixed
Close, 80 DEG C of stirring ultrasonic reactions for 24 hours, after reaction, cooled to room temperature and still aging 12h.The production that reaction is obtained
Object centrifuge separation, discards clarified solution, the sediment left, uses deionized water and ethanol washing 3 times respectively, and ultrasonic disperse is dry,
Obtain sulfaquinoxaline nickel micro particles.The product is observed with scanning electron microscope (SEM) referring to Fig. 1, and product is granular micro-
Grain, size is about 300~800nm.
Embodiment 3
Ethanol solution each 50mL of the nickel chloride aqueous solution and 10mmol/L sodium sulfaquinoxaline of 10mmol/L is prepared, it is standby
With；
The nickel chloride aqueous solution of 5mL 10mmol/L and the ethanol solution of 5mL 10mmol/L sodium sulfaquinoxaline are taken respectively
Mixing, 60 DEG C of stirring ultrasonic reaction 20h, cooled to room temperature and still aging 20h.The product centrifugation point that reaction is obtained
From discarding clarified solution, the sediment left uses deionized water and ethanol washing 3 times respectively, and ultrasonic disperse is dry, i.e. acquisition sulphur
Amine quinoxaline nickel micro particles.The product is observed with scanning electron microscope (SEM) referring to Fig. 1, and product is granular particle, and size is big
Small 300~800nm.
Embodiment 4
Methanol solution each 50mL of the nickel acetate aqueous solution and 10mmol/L sodium sulfaquinoxaline of 20mmol/L is prepared, it is standby
With；
The aqueous solution of the nickel acetate aqueous solution and 5mL 10mmol/L sodium sulfaquinoxaline that take 5mL 20mmol/L respectively is mixed
It closes, 50 DEG C of stirring ultrasonic reaction 12h, cooled to room temperature is simultaneously aged for 24 hours.The product centrifuge separation that reaction is obtained, discards
Clarified solution, the sediment left use deionized water and ethanol washing 3 times respectively, and ultrasonic disperse is dry, i.e. acquisition sulfanilamide (SN) quinoline is disliked
Quinoline nickel micro particles.Fig. 1 is shown in the product scanning electron microscope (SEM) observation, and product is granular particle, size 300~
800nm。
With embodiment 1, embodiment 2, embodiment 3, embodiment 4, the sulfaquinoxaline nickel micro-and nano-particles of preparation, which are used as, is urged
Agent carries out catalysis reaction:
The sulfaquinoxaline nickel micro-and nano-particles prepared using above-described embodiment 1 are that catalyst carries out catalysis reaction, are reacted
Condition are as follows: will to iodobenzene ether (1.0mmol), to methylphenylboronic acid (1.1mmol), K2CO3Prepared by (2.0mmol) and example 1
Sulfaquinoxaline nickel micro particles catalyst (30mg) be fitted into the heavy wall pressure bottle of 25mL, reaction dissolvent EtOH/H2O
The mixed solution of (3mL/4mL) is stirred to react for 24 hours at 90 DEG C.Later, (10mL × 3), saturated salt solution is extracted with ethyl acetate
It washs (10mL × 2), anhydrous sodium sulfate is dry, and organic phase is removed under reduced pressure, using column chromatography separation product, obtains white solid powder
End, yield 90%.It is as follows to react skeleton symbol:
The micro-nano particle of sulfaquinoxaline nickel prepared using above-described embodiment 1 is that catalyst carries out catalysis reaction, is reacted
Condition are as follows: by para-bromoanisole (1.0mmol), phenyl boric acid (1.1mmol), K2CO3Sulfanilamide (SN) prepared by (2.0mmol) and example 1
Quinoxaline nickel micro particles catalyst (33mg) is fitted into the single-necked flask of 25mL, reaction dissolvent EtOH/H2O(3mL/6mL)
Mixed solution, stirred for 24 hours at 90 DEG C.Later, it is extracted with ethyl acetate (10mL × 3), saturated common salt water washing (10mL ×
2), anhydrous sodium sulfate is dry, and organic phase is removed under reduced pressure, using column chromatography separation product, obtains white solid powder, yield is
80%.It is as follows to react skeleton symbol:
The micro-nano particle of sulfaquinoxaline nickel prepared using above-described embodiment 1 is that catalyst carries out catalysis reaction, is reacted
Condition are as follows: will to iodobenzene ether (1.0mmol), to fluorobenzoic boric acid (1.1mmol), K2CO3Prepared by (2.0mmol) and example 1
Sulfaquinoxaline nickel micro particles catalyst (33mg) is fitted into the heavy wall pressure bottle of 25mL, reaction dissolvent EtOH/H2O
The mixed solution of (3mL/6mL) stirs for 24 hours at 90 DEG C.Later, it is extracted with ethyl acetate (10mL × 3), saturated common salt washing
It washs (10mL × 2), anhydrous sodium sulfate is dry, and organic phase is removed under reduced pressure, using column chromatography separation product, obtains white solid powder
End, yield 95%.It is as follows to react skeleton symbol:
The micro-nano particle of sulfaquinoxaline nickel prepared using above-described embodiment 2 is that catalyst carries out catalysis reaction, is reacted
Condition are as follows: will to iodobenzene ether (1.0mmol), to methylphenylboronic acid (1.1mmol), K2CO3Prepared by (2.0mmol) and example 2
Sulfaquinoxaline nickel micro particles catalyst (30mg) be fitted into the heavy wall pressure bottle of 25mL, reaction dissolvent EtOH/H2O
The mixed solution of (3mL/6mL) stirs for 24 hours at 90 DEG C.Later, it is extracted with ethyl acetate (10mL × 3), saturated common salt washing
It washs (10mL × 2), anhydrous sodium sulfate is dry, and organic phase is removed under reduced pressure, using column chromatography separation product, obtains white solid powder
End, yield 92%.It is as follows to react skeleton symbol:
The micro-nano particle of sulfaquinoxaline nickel prepared using above-described embodiment 3 is that catalyst carries out catalysis reaction, is reacted
Condition are as follows: will to iodobenzene ether (1.0mmol), to methylphenylboronic acid (1.1mmol), K2CO3Prepared by (2.0mmol) and example 3
Sulfaquinoxaline nickel micro particles catalyst (30mg) be fitted into the heavy wall pressure bottle of 25mL, reaction dissolvent EtOH/H2O
The mixed solution of (3mL/6mL) stirs for 24 hours at 90 DEG C.Later, it is extracted with ethyl acetate (10mL × 3), saturated common salt washing
It washs (10mL × 2), anhydrous sodium sulfate is dry, and organic phase is removed under reduced pressure, using column chromatography separation product, obtains white solid powder
End, yield 89%.It is as follows to react skeleton symbol:
The micro-nano particle of sulfaquinoxaline nickel prepared using above-described embodiment 4 is that catalyst carries out catalysis reaction, is reacted
Condition are as follows: will to iodobenzene ether (1.0mmol), to methylphenylboronic acid (1.1mmol), K2CO3Prepared by (2.0mmol) and example 4
Sulfaquinoxaline nickel micro particles catalyst (30mg) be fitted into the heavy wall pressure bottle of 25mL, reaction dissolvent EtOH/H2O
The mixed solution of (3mL/6mL) stirs for 24 hours at 90 DEG C.Later, it is extracted with ethyl acetate (10mL × 3), saturated common salt washing
It washs (10mL × 2), anhydrous sodium sulfate is dry, and organic phase is removed under reduced pressure, using column chromatography separation product, obtains white solid powder
End, yield 93%.It is as follows to react skeleton symbol:
It should be understood by those ordinary skilled in the art that: the above is only a specific embodiment of the present invention, and
It is not used in the limitation present invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done,
It should be included within protection scope of the present invention.
Claims (2)
1. a kind of preparation method of nickel micro-and nano-particles, which is characterized in that preparation method includes:
It weighs sodium sulfaquinoxaline to be dissolved in solvent, obtains sulfaquinoxaline sodium salt solution；
It is soluble in water to weigh nickel salt, obtains nickel salt aqueous solution；
Prepared nickel salt aqueous solution is added in sulfaquinoxaline sodium salt solution, at 20~80 DEG C ultrasonic reaction 12~
For 24 hours, wherein initial Ni2+It is 1:0.5~3 with the ratio between the amount of substance of sulfaquinoxaline；After reaction, still aging 12~
24h；
By the product centrifuge separation after ageing, sediment is left, respectively the sediment described in deionized water and ethanol washing, ultrasound
Dispersion, it is dry, that is, obtain sulfaquinoxaline nickel micro-and nano-particles；
The nickel salt is selected from one or more of nickel sulfate, nickel chloride, nickel acetate；
The partial size of the nickel micro-and nano-particles is 300~800nm.
2. nickel micro-and nano-particles made from preparation method according to claim 1, which is characterized in that the nickel micro-nano grain of rice
Son is graininess, for being catalyzed C-C coupling reaction.
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| CN105949134B (en) * | 2016-04-29 | 2018-07-20 | 宁波大学 | A kind of sulphadiazine iron palladium nano-complex particle and preparation method thereof |
| CN105944761B (en) * | 2016-04-29 | 2018-06-15 | 宁波大学 | A kind of sulfaquinoxaline cobalt nickel nanocomposite and preparation method thereof |
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| DE10300098A1 (en) * | 2003-01-07 | 2004-07-15 | Bayer Ag | Copper-carbene complexes and their use |
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| CN101912975A (en) * | 2009-11-29 | 2010-12-15 | 宁波大学 | Method for preparing ultrahigh monodisperse nickel sol by using novel protective agent |
| CN103170649A (en) * | 2013-04-15 | 2013-06-26 | 南京理工大学 | Preparation method of magnetic nickel nano material |
| CN103396356A (en) * | 2013-08-12 | 2013-11-20 | 宁波大学 | Spirofluorene copper pyridine micro-nano particle and preparation method thereof |
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