CN104668577A - Nickel micro nanoparticle and preparation method thereof - Google Patents
Nickel micro nanoparticle and preparation method thereof Download PDFInfo
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- CN104668577A CN104668577A CN201510060567.2A CN201510060567A CN104668577A CN 104668577 A CN104668577 A CN 104668577A CN 201510060567 A CN201510060567 A CN 201510060567A CN 104668577 A CN104668577 A CN 104668577A
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Abstract
The invention discloses a nickel micro nanoparticle and a preparation method thereof. The preparation method comprises the following steps: adding a certain quantity of nickel salt solution into a solution which contains sodium sulfaquinoxaline, performing centrifugation on products after reaction and aging at a certain temperature, leaving precipitate, washing the precipitate respectively with deionized water and ethanol, performing ultrasonic dispersion, and drying, so as to prepare the corresponding sulfaquinoxaline nickel micro nanoparticle. According to the preparation method, the preparation of metal micro nanoparticles through reaction to different nickel salts and sulfaquinoxaline is successfully realized, metal-ligand micro nanoparticles with uniform particle size are obtained, and excellent physical and chemical properties are provided. The sulfaquinoxaline nickel micro nanoparticle as a catalyst has good catalytic activity and wide application prospects in the field of catalysis. In a whole preparation process, the operation is simple, the cost of raw materials is low, the equipment investment is low, and mass production is facilitated.
Description
Technical field
The present invention relates to micro-nano material field, refer to a kind of nickel micro-and nano-particles and preparation method thereof especially.
Background technology
Nanometer technology is as a kind of emerge science technology most with market application potential, and its potential importance is unquestionable, and some developed countries all drop into a large amount of funds and carry out research work.As colonial has set up research in nanotechnology center, portion of Japanese culture and education section is nanometer technology, and at home, many scientific research institutions, institution of higher learning also organize scientific research strength to one of four large primary study exploration projects being classified as material science, carry out the research work of nanometer technology.
Nano particle also makes ultramicro powder be the transitional region being in cluster and macro object boundary, such system is atypical microscopic system also atypical macrosystem both, be a kind of typical Mesoscopic structure, it has skin effect, small-size effect and macro quanta tunnel effect.After macro object is subdivided into ultramicro powder (nanoscale) by people, it will demonstrate many unusual characteristics, namely will have significant difference when the character of its rare earth nano material optics, calorifics, electricity, magnetics, mechanics and chemical aspect is compared with bulk solid, greatly develop new and high technology new product.Therefore nano material is used for the aspects such as heat-barrier material, semiconductor, catalyst very high development prospect.Especially for the configuration of surface of nano-corpuscule, along with the reduction of particle diameter, smooth surface degree reduces, and defines scraggly atomic steps, this adds increased the contact surface of chemical reaction, thus improve the effective rate of utilization of catalyst.
For nickel micro Nano material catalyzed coupling reaction, also there is some problems needs to go to solve.
First, the organic chemist research nickel micro Nano material catalytic performance of specialty is concrete not enough, need to improve to the catalytic selectivity of differential responses substrate.Whether the structure of nickel micro Nano material, the factor such as size and pattern can be impacted catalytic performance, do not carry out the research that system is deep, more do not propose how to design the micro-nano catalyst of nickel to improve the efficiency of catalyzed coupling reaction.
Secondly, nickel micro Nano material is compared with palladium catalyst, and catalytic activity is not high.Therefore, significantly improving the catalytic activity of catalyst, reduce the consumption of catalyst, is also one of major issue of current needs solution.
Summary of the invention
In view of this, the object of the invention is to propose a kind of reaction condition gentle, preparation process is simple, with low cost, nickel micro-and nano-particles simultaneously with good catalytic and preparation method thereof.
Based on above-mentioned purpose nickel micro-and nano-particles provided by the invention and preparation method thereof, specifically comprise the following steps:
Taking Embazin is dissolved in solvent, obtains sulfaquinoxaline sodium salt solution;
Take nickel salt soluble in water, obtain nickel salt aqueous solution;
Prepared nickel salt aqueous solution is joined in sulfaquinoxaline sodium salt solution, ultrasonic reaction 12 ~ 24h at 20 ~ 80 DEG C, wherein initial Ni
2+be 1:0.5 ~ 3 with the ratio of Embazin amount of substance; After reaction terminates, still aging 12 ~ 24h;
By the product centrifugation after ageing, leave sediment, wash described sediment, ultrasonic disperse with deionized water and ethanol respectively, dry, namely obtain described sulfaquinoxaline nickel micro-and nano-particles.
Alternatively, described Embazin, its molecular formula is C
14h
11n
4naO
2s, structural formula is:
Alternatively, described solvent is one or more in ethanol, methyl alcohol, water.
Alternatively, described nickel salt is divalent nickel salt, is selected from one or more in nickelous sulfate, nickel chloride, nickel nitrate and nickel acetate.
The invention provides a kind of sulfaquinoxaline nickel micro-and nano-particles and be used as catalyst, described sulfaquinoxaline nickel micro-and nano-particles particle diameter is 300 ~ 5000nm, for catalysis C-C coupling reaction.
As can be seen from above, 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 selected.
2. nickel micro-and nano-particles described in has unique structure and has 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, environmental protection.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of embodiment of the present invention nickel micro-and nano-particles.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
Embodiment 1
The nickel sulfate solution of preparation 5mmol/L and each 50mL of 15mmol/L sulfaquinoxaline sodium water solution, for subsequent use;
Get the nickel sulfate solution of 5mL 5mmol/L and the aqueous solution of 5mL 15mmol/L Embazin respectively, 20 DEG C are stirred ultrasonic reaction 24h, after reaction terminates, and still aging 12h.By the product centrifugation that reaction obtains, discard clarified solution, the sediment stayed, wash 3 times, ultrasonic disperse with deionized water and ethanol respectively, dry, namely obtain sulfaquinoxaline nickel micro particles.This product ESEM (SEM) is observed see Fig. 1, and product is granular particulate, and size is about 300 ~ 800nm.
Embodiment 2
The nickel nitrate aqueous solution of preparation 10mmol/L and each 50mL of 10mmol/L sulfaquinoxaline sodium water solution, for subsequent use;
Get the nickel sulfate solution of 5mL 10mmol/L and the aqueous solution of 5mL 10mmol/L Embazin respectively, 80 DEG C are stirred ultrasonic reaction 24h, after reaction terminates, naturally cool to room temperature and still aging 12h.By the product centrifugation that reaction obtains, discard clarified solution, the sediment stayed, wash 3 times, ultrasonic disperse with deionized water and ethanol respectively, dry, namely obtain sulfaquinoxaline nickel micro particles.This product ESEM (SEM) is observed see Fig. 1, and product is granular particulate, and size is about 300 ~ 800nm.
Embodiment 3
The preparation nickel chloride aqueous solution of 10mmol/L and each 50mL of ethanolic solution of 10mmol/L Embazin, for subsequent use;
Get the nickel chloride aqueous solution of 5mL 10mmol/L and the ethanolic solution mixing of 5mL 10mmol/L Embazin respectively, 60 DEG C are stirred ultrasonic reaction 20h, naturally cool to room temperature and still aging 20h.By the product centrifugation that reaction obtains, discard clarified solution, the sediment stayed, wash 3 times, ultrasonic disperse with deionized water and ethanol respectively, dry, namely obtain sulfaquinoxaline nickel micro particles.This product ESEM (SEM) is observed see Fig. 1, and product is granular particulate, size 300 ~ 800nm.
Embodiment 4
The preparation nickel acetate aqueous solution of 20mmol/L and each 50mL of methanol solution of 10mmol/L Embazin, for subsequent use;
Get the nickel acetate aqueous solution of 5mL 20mmol/L and the aqueous solution of 5mL 10mmol/L Embazin respectively, 50 DEG C are stirred ultrasonic reaction 12h, naturally cool to room temperature and ageing 24h.By the product centrifugation that reaction obtains, discard clarified solution, the sediment stayed, wash 3 times, ultrasonic disperse with deionized water and ethanol respectively, dry, namely obtain sulfaquinoxaline nickel micro particles.This product ESEM (SEM) is observed and is seen Fig. 1, and product is granular particulate, size 300 ~ 800nm.
With embodiment 1, embodiment 2, embodiment 3, embodiment 4, the sulfaquinoxaline nickel micro-and nano-particles of preparation, as catalyst, carries out catalytic reaction:
The sulfaquinoxaline nickel micro-and nano-particles using above-described embodiment 1 to prepare carries out catalytic reaction for catalyst, and reaction condition is: will to iodobenzene ether (1.0mmol), to methylphenylboronic acid (1.1mmol), K
2cO
3(2.0mmol) sulfaquinoxaline nickel micro particles catalyst (30mg) and prepared by example 1 loads in the heavy wall pressure bottle of 25mL, and reaction dissolvent is EtOH/H
2the mixed solution of O (3mL/4mL), stirring reaction 24h at 90 DEG C.Afterwards, be extracted with ethyl acetate (10mL × 3), saturated common salt water washing (10mL × 2), anhydrous sodium sulfate drying, decompression removing organic phase, adopt column chromatography separated product, obtain white solid powder, productive rate is 90%.Reaction skeleton symbol is as follows:
The micro-nano particulate of sulfaquinoxaline nickel using above-described embodiment 1 to prepare carries out catalytic reaction for catalyst, and reaction condition is: by para-bromoanisole (1.0mmol), phenyl boric acid (1.1mmol), K
2cO
3(2.0mmol) sulfaquinoxaline nickel micro particles catalyst (33mg) and prepared by example 1 loads in the single port flask of 25mL, and reaction dissolvent is EtOH/H
2the mixed solution of O (3mL/6mL), stirs 24h at 90 DEG C.Afterwards, be extracted with ethyl acetate (10mL × 3), saturated common salt water washing (10mL × 2), anhydrous sodium sulfate drying, decompression removing organic phase, adopt column chromatography separated product, obtain white solid powder, productive rate is 80%.Reaction skeleton symbol is as follows:
The micro-nano particulate of sulfaquinoxaline nickel using above-described embodiment 1 to prepare carries out catalytic reaction for catalyst, and reaction condition is: will to iodobenzene ether (1.0mmol), to fluorobenzoic boric acid (1.1mmol), K
2cO
3(2.0mmol) sulfaquinoxaline nickel micro particles catalyst (33mg) and prepared by example 1 loads in the heavy wall pressure bottle of 25mL, and reaction dissolvent is EtOH/H
2the mixed solution of O (3mL/6mL), stirs 24h at 90 DEG C.Afterwards, be extracted with ethyl acetate (10mL × 3), saturated common salt water washing (10mL × 2), anhydrous sodium sulfate drying, decompression removing organic phase, adopt column chromatography separated product, obtain white solid powder, productive rate is 95%.Reaction skeleton symbol is as follows:
The micro-nano particulate of sulfaquinoxaline nickel using above-described embodiment 2 to prepare carries out catalytic reaction for catalyst, and reaction condition is: will to iodobenzene ether (1.0mmol), to methylphenylboronic acid (1.1mmol), K
2cO
3(2.0mmol) sulfaquinoxaline nickel micro particles catalyst (30mg) and prepared by example 2 loads in the heavy wall pressure bottle of 25mL, and reaction dissolvent is EtOH/H
2the mixed solution of O (3mL/6mL), stirs 24h at 90 DEG C.Afterwards, be extracted with ethyl acetate (10mL × 3), saturated common salt water washing (10mL × 2), anhydrous sodium sulfate drying, decompression removing organic phase, adopt column chromatography separated product, obtain white solid powder, productive rate is 92%.Reaction skeleton symbol is as follows:
The micro-nano particulate of sulfaquinoxaline nickel using above-described embodiment 3 to prepare carries out catalytic reaction for catalyst, and reaction condition is: will to iodobenzene ether (1.0mmol), to methylphenylboronic acid (1.1mmol), K
2cO
3(2.0mmol) sulfaquinoxaline nickel micro particles catalyst (30mg) and prepared by example 3 loads in the heavy wall pressure bottle of 25mL, and reaction dissolvent is EtOH/H
2the mixed solution of O (3mL/6mL), stirs 24h at 90 DEG C.Afterwards, be extracted with ethyl acetate (10mL × 3), saturated common salt water washing (10mL × 2), anhydrous sodium sulfate drying, decompression removing organic phase, adopt column chromatography separated product, obtain white solid powder, productive rate is 89%.Reaction skeleton symbol is as follows:
The micro-nano particulate of sulfaquinoxaline nickel using above-described embodiment 4 to prepare carries out catalytic reaction for catalyst, and reaction condition is: will to iodobenzene ether (1.0mmol), to methylphenylboronic acid (1.1mmol), K
2cO
3(2.0mmol) sulfaquinoxaline nickel micro particles catalyst (30mg) and prepared by example 4 loads in the heavy wall pressure bottle of 25mL, and reaction dissolvent is EtOH/H
2the mixed solution of O (3mL/6mL), stirs 24h at 90 DEG C.Afterwards, be extracted with ethyl acetate (10mL × 3), saturated common salt water washing (10mL × 2), anhydrous sodium sulfate drying, decompression removing organic phase, adopt column chromatography separated product, obtain white solid powder, productive rate is 93%.Reaction skeleton symbol is as follows:
Those of ordinary skill in the field are to be understood that: the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. a preparation method for nickel micro-and nano-particles, is characterized in that, preparation method comprises:
Taking Embazin is dissolved in solvent, obtains sulfaquinoxaline sodium salt solution;
Take nickel salt soluble in water, obtain nickel salt aqueous solution;
Prepared nickel salt aqueous solution is joined in sulfaquinoxaline sodium salt solution, ultrasonic reaction 12 ~ 24h at 20 ~ 80 DEG C, wherein initial Ni
2+be 1:0.5 ~ 3 with the ratio of the amount of substance of sulfaquinoxaline; After reaction terminates, still aging 12 ~ 24h;
By the product centrifugation after ageing, leave sediment, wash described sediment, ultrasonic disperse with deionized water and ethanol respectively, dry, namely obtain sulfaquinoxaline nickel micro-and nano-particles.
2. the preparation method of nickel micro-and nano-particles according to claim 1, is characterized in that, selected nickel salt is divalent nickel salt, is selected from one or more in nickelous sulfate, nickel chloride, nickel acetate.
3. the preparation method of nickel micro-and nano-particles according to claim 1, is characterized in that, described nickel micro-and nano-particles is graininess, and particle diameter is 300 ~ 800nm.
4. the preparation method of nickel micro-and nano-particles according to claim 1, is characterized in that, described nickel micro-and nano-particles is graininess, and particle diameter is 300 ~ 800nm, catalysis C-C coupling reaction.
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Cited By (2)
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| CN105949134A (en) * | 2016-04-29 | 2016-09-21 | 宁波大学 | Sulfadiazine iron palladium nano-composite particle and preparation method thereof |
| CN105944761A (en) * | 2016-04-29 | 2016-09-21 | 宁波大学 | Sulfaquinoxaline cobalt-nickel nano composite material and preparation method thereof |
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Cited By (4)
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| CN105949134A (en) * | 2016-04-29 | 2016-09-21 | 宁波大学 | Sulfadiazine iron palladium nano-composite particle and preparation method thereof |
| CN105944761A (en) * | 2016-04-29 | 2016-09-21 | 宁波大学 | Sulfaquinoxaline cobalt-nickel nano composite material 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 |
| 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 |
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