CN103433044A - Preparation method of cobalt-nickel double metal hydroxide nano composite - Google Patents

Preparation method of cobalt-nickel double metal hydroxide nano composite Download PDF

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CN103433044A
CN103433044A CN2013104008898A CN201310400889A CN103433044A CN 103433044 A CN103433044 A CN 103433044A CN 2013104008898 A CN2013104008898 A CN 2013104008898A CN 201310400889 A CN201310400889 A CN 201310400889A CN 103433044 A CN103433044 A CN 103433044A
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cobalt
nickel
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CN103433044B (en
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宋吉明
倪晶晶
张洁
张胜义
牛和林
毛昌杰
沈玉华
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Guangdong Branch Road heat source technology Co. Ltd.
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Anhui University
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Abstract

The invention provides a method for preparing a cobalt-nickel double metal hydroxide nano composite through a hydrolytic process, belonging to the technical field of nano material preparation. The method is carried out under the condition of room temperature, dispenses with heating and temperature control devices and takes distilled water as a solvent, hydrolysis of sodium borohydride is utilized to provide an alkaline environment for reaction, the synthetic steps are simple, the yield is high and the obtained cobalt-nickel double metal hydroxide nano composite is a grapheme-like structure. The method is simple and energy-saving in preparation process and is suitable for industrial production. The obtained cobalt-nickel double metal hydroxide nano composite has good catalytic effects on hydrogenation of p-nitrophenol.

Description

The preparation method of a kind of cobalt-nickel bimetal hydroxide nanometer complexes
Technical field:
The invention belongs to the nano material preparing technical field, be specifically related to adopt at ambient temperature hydrolysis to prepare class graphene-like cobalt-nickel bimetal hydroxide nanometer complexes, this nano-complex has the character of efficient catalytic p-nitrophenol hydrogenation.
Background technology:
The existing method for preparing cobalt-nickel bimetal hydroxide nanometer complexes comprises self-assembling technique, electrodeposition process, coprecipitation, template, microemulsion method, sol-gel process etc.
Holland's " energy magazine " (Journal of Power Sources,, 172 volumes, 970-974 page in 2007) reported and first adopted ammonia precipitation method preparation to take the α-Co (OH) of the one dimension stratiform that the dodecyl sulphate root is interlayer 2and α-Ni (OH) 2, then they are dispersed in n-butanol and form colloidal solution, in latter two colloidal solution, by self-assembling technique, pile up altogether at random, obtained having the α-hydroxide nanometer complexes of stable electrical chemical property.Similar with the method, Holland's " investigation of materials communique " (Materials Research Bulletin,, 48 volumes, 2715-2719 page in 2013) reported and first made to take α-Co (OH) that both sexes p-aminobenzoic acid radical ion is interlayer 2and α-Ni (OH) 2peel off in water, add excessive nitrate ion to disperse in mixed system to the colloid of the two, through ion-exchange, α-Co (OH) 2and α-Ni (OH) 2all become nitrate ion between interlayer, last α-Co (OH) 2and α-Ni (OH) 2form stratiform α-hydroxide nanometer complexes by piling up altogether.Holland " energy magazine " (Journal of Power Sources, 2008,175 volumes, the 680-685 page) reported and usingd cabaltous nitrate hexahydrate and Nickelous nitrate hexahydrate as He Nie source, cobalt source predecessor, take Ag/AgCl as reference electrode in three-electrode system, stainless-steel sheet is working electrode, in KOH solution, uses permanent electromotive force sedimentation to prepare Co xni 1-xlayered double-hydroxide, have higher ratio capacitance.Holland " electrochemistry journal " (Electrochimica Acta, 2009,54 volumes, the 2737-2741 page) reported the employing chemical coprecipitation method, using cabaltous nitrate hexahydrate and Nickelous nitrate hexahydrate as He Nie source, cobalt source predecessor, in the aqueous solution, add polyethylene glycol as structure directing agent, and add certain density ammoniacal liquor regulator solution pH value, synthesized a kind of mesoporous Co xni 1-xlayered double-hydroxide.Britain's " materials chemistry magazine " (Journal of Materials Chemistry,, 22 volumes, 23587-23592 page in 2012) has reported by using synthetic SiO in early stage 2@AlOOH is template, is adding cabaltous nitrate hexahydrate, and after Nickelous nitrate hexahydrate and urea, original position is synthetic has inner hollow, the nickel that outside is the three-dimensional structure of class hedgehog shell-cobalt double-hydroxide microballoon.The special construction of this hydroxide has effectively improved faradic redox reaction and mass transport process in electrochemical process.Holland " applied catalysis B: environment " (Applied Catalysis B:Environmental, 2013, the 136-137 volume, the 1-8 page) reported and usingd six hydration nickel sulfate and Cobalt monosulfate heptahydrate respectively as He Gu source, nickel source predecessor, adopt loaded Catalyst By Water-in-oil Microemulsion to synthesize a kind of nickel-cobalt hydroxide nanometer sheet on carbon base body, and study its catalytic action to evolving hydrogen reaction as electrode material.Britain's " chemical communication " (Chemical Communication,, 49 volumes, 7067-7069 page in 2013) reported and usingd cabaltous nitrate hexahydrate and Nickelous nitrate hexahydrate as He Nie source, cobalt source predecessor, the lithium hydroxide (LiOH) of take is precipitating reagent, azanol (NH 2oH) be complexing agent, adopt coprecipitation method at titanium plate Surface Creation a kind of cobalt-nickel multi-phase composites.Holland " energy magazine " (Journal of Power Sources, 2013,238 volumes, 180-189 page) reported that usining Nickel dichloride hexahydrate and cobalt chloride hexahydrate synthesizes a kind of nickel-cobalt hydroxide as He Gu source, nickel source predecessor by sol-gel process.
In sum, it is also less that cobalt-nickel bimetal hydroxide is studied aspect simple synthesis, and its application is to study its electrochemical properties as electrode material mostly, and application in other respects is less.Particularly as catalyst, the application in solution system also is not in the news at present.
Summary of the invention:
The objective of the invention is to propose preparation method and the application aspect the hydrogenation of catalysis p-nitrophenol thereof of a kind of cobalt-nickel bimetal hydroxide nanometer complexes.This method preparation process is simple, energy-conservation, is applicable to suitability for industrialized production, and the cobalt obtained-nickel bimetal hydroxide nanometer complexes is class Graphene stratiform structure, and thickness, less than 1 nanometer, has the character of efficient catalytic p-nitrophenol hydrogenation.In addition, because product has ferromagnetism, be easy to separated and collect with magnet, be conducive to its recycling in catalysis p-nitrophenol hydrogenation experiment.
The preparation method of cobalt of the present invention-nickel bimetal hydroxide nanometer complexes comprises the following steps:
The cabaltous nitrate hexahydrate of A, weighing 0.146 gram and 0.200 gram polyvinylpyrrolidone (PVP) ultrasonic dissolution, in 40 ml distilled waters, then are transferred to three-neck flask, open the rotating speed agitating solution that electric blender arranges 1000 rev/mins.
B, under stirring condition, drip 40 milliliters of new configuration with syringe pump containing 0.750 gram sodium borohydride aqueous solution, within 15 minutes, drip.Subsequently, with syringe pump, drip 40 milliliters containing the 0.119 gram Nickel dichloride hexahydrate aqueous solution, within 15 minutes, drip.
After C, all reagent add, solution continues stirring reaction one hour, after reaction finishes, by solution centrifugal, collects the black solid product, with distilled water and ethanol, respectively washs three times, 60 degrees centigrade of oven dry, obtains sample.
The experimental technique of catalysis p-nitrophenol hydrogenation comprises: by the p-nitrophenyl phenol solution of 0.1 milliliter of 0.004M, 2 ml distilled waters, the freshly prepd sodium borohydride solution of 1 milliliter of 0.1M is added in quartz colorimetric utensil in order successively, the color of solution is immediately by the light yellow glassy yellow that becomes, simultaneously absworption peak by 317 nanometer red shifts to 400 nanometers left and right, add subsequently the cobalt of 1 milligram of preparation-nickel bimetal hydroxide nanometer complexes, with ultraviolet specrophotometer, between the 200-500 nanometer, every 1 minute, test once, until dropping to no longer, the absworption peak peak value of 400 nanometers changes.Result shows, at ambient temperature, the cobalt of 1 milligram of preparation-nickel bimetal hydroxide nanometer complexes only needs 6 minutes just can be complete by the p-nitrophenol solution catalyzing of 0.1 milliliter of 0.004M.
The invention provides and a kind ofly be hydrolyzed by sodium borohydride the method that provides alkaline environment to prepare cobalt-nickel bimetal hydroxide nanometer complexes and in the application aspect the hydrogenation of catalysis p-nitrophenol in the aqueous solution, this reaction is at room temperature carried out, the decomposition of sodium borohydride provides alkaline environment, polyvinylpyrrolidone (PVP) is as stabilizing agent, the course of reaction gentleness, be easy to control.In addition prepared sample has certain ferromagnetism, can be separated with magnet easily and collect.
Cobalt prepared by the present invention-nickel bimetal hydroxide nanometer complexes is under the protection of stabilizing agent, by sodium borohydride, is decomposed and to be provided alkaline environment, He Nie source, cobalt source to generate successively that then corresponding hydroxide be compounded to form.The kind of stabilizing agent and institute's consumption all have a certain impact to the pattern of product.
Described cobalt source predecessor is cabaltous nitrate hexahydrate;
Described nickel source predecessor is Nickel dichloride hexahydrate;
Described reaction temperature is room temperature (25 ℃);
Described reaction vessel is three-neck flask;
Described solvent is distilled water;
Described stabilizing agent is polyvinylpyrrolidone (PVP);
Described agitating device is electric blender;
Described mixing speed is 1000 rev/mins.
Cobalt prepared by the present invention-nickel bimetal hydroxide nanometer complexes, to the catalysis nitrophenol, hydrogenation has good effect to this sample, as the p-nitrophenyl phenol solution by 0.1 milliliter of 0.004M, 2 ml distilled waters are added in quartz colorimetric utensil in order successively, pass through measurement of ultraviolet-visible spectrophotometer, in 317 nanometers, one absworption peak is arranged, this peak is the ultraviolet absorption peak of p-nitrophenol, after adding again the freshly prepd sodium borohydride solution of 1 milliliter of 0.1M, solution is immediately by the light yellow glassy yellow that becomes, simultaneously ultraviolet absorption peak by 317 nanometer red shifts to 400 nanometers, the generation of this phenomenon is to make the solution alkalize because the sodium borohydride added decomposes, can in and p-nitrophenol in hydroxyl, thereby form the p-nitrophenol ion, and 400 nanometers appearance is the ultraviolet absorption peak of p-nitrophenol ion, the corresponding concentration of this absworption peak is decided to be to initial concentration.Finally, to the cobalt that adds 1 milligram of preparation in cuvette-nickel bimetal hydroxide nanometer complexes, every one minute, use measurement of ultraviolet-visible spectrophotometer, change until the absworption peak peak value of 400 nanometers drops to no longer.Simultaneously, along with the decline of 400 nanometers absworption peak peak values, in 300 nanometers, occurred that new absworption peak and peak value constantly increase, this is the feature ultraviolet absorption peak of para-aminophenol ion.In addition, the amount of the concentration of sodium borohydride, catalyst also has a great impact the speed of catalysis p-nitrophenol hydrogenation.
The reducing agent of described catalysis p-nitrophenol hydrogenation is freshly prepd sodium borohydride;
Describedly treat that the catalysis sample is p-nitrophenol;
Described ultraviolet specrophotometer is Shimadzu UV-1750 ultraviolet specrophotometer.
In a word, the cobalt that prepared by the present invention-nickel bimetal hydroxide nanometer complexes has the character of efficient catalytic p-nitrophenol hydrogenation.Simultaneously, because this material has ferromagnetism, can very convenient separation and the collection of carrying out product with magnet, be conducive to reusing of material.Therefore, this material has potential using value at catalytic field.
The accompanying drawing explanation:
The scanning electron microscope (SEM) photograph (SEM) that Fig. 1, Fig. 2 are the cobalt for preparing by hydrolysis under room temperature in embodiment 1-nickel bimetal hydroxide nanometer complexes;
The transmission electron microscope picture (TEM) that Fig. 3, Fig. 4 are the cobalt for preparing in embodiment 1-nickel bimetal hydroxide nanometer complexes;
The X-ray powder diffraction figure (XRD) that Fig. 5 is the cobalt for preparing in embodiment 1-nickel bimetal hydroxide nanometer complexes;
The hysteresis curve that Fig. 6 is the cobalt for preparing in embodiment 1-nickel bimetal hydroxide nanometer complexes;
The ultraviolet-ray visible absorbing curve that Fig. 7, Fig. 8 are the cobalt for preparing in embodiment 2-nickel bimetal hydroxide nanometer complexes catalysis p-nitrophenol hydrogenation.
The specific embodiment:
Below in conjunction with embodiment, the present invention is done to specific description.
Embodiment 1: preparation class graphene-like cobalt-nickel bimetal hydroxide nanometer complexes:
The cabaltous nitrate hexahydrate of A, weighing 0.146 gram and 0.200 gram polyvinylpyrrolidone (PVP) ultrasonic dissolution, in 40 ml distilled waters, then are transferred to three-neck flask, open the rotating speed agitating solution that electric blender arranges 1000 rev/mins.
B, under stirring condition, drip 40 milliliters of new configuration with syringe pump containing 0.750 gram sodium borohydride aqueous solution, within 15 minutes, drip.Subsequently, with syringe pump, drip 40 milliliters containing the 0.119 gram Nickel dichloride hexahydrate aqueous solution, within 15 minutes, drip.
After C, all reagent add, solution continues stirring reaction one hour, after reaction finishes products therefrom after distilled water and three centrifuge washings of ethanol 60 degrees centigrade of oven dry, for characterizing and test.
Adopt the field emission electron flying-spot microscope JSM-6700F of NEC (SEM) and the JEM-2100 of NEC high resolution transmission electron microscopy (HRTEM) to carry out morphology characterization to the sample obtained.Adopt Philip X'Pert PRO SUPER X-ray diffractometer (XRD) to characterize the sample phase.
Fig. 1, Fig. 2 are in embodiment 1, and the SEM of the cobalt prepared by hydrolysis under room temperature-nickel bimetal hydroxide nanometer complexes schemes, and can find out the pattern homogeneous of product, are the accordion class graphene-structured be comprised of nanometer sheet; Fig. 3 Fig. 4 is in embodiment 1, and the TEM figure of the cobalt prepared by hydrolysis under room temperature-nickel bimetal hydroxide nanometer complexes, can find out that product is comprised of very thin nanometer sheet, and the thickness of nanometer sheet is about 1 nanometer;
Fig. 5 is in embodiment 1, and the XRD figure of the cobalt prepared by hydrolysis under room temperature-nickel bimetal hydroxide nanometer complexes, can find out in sample and contain α-Co (OH) 2and α-Ni (OH) 2;
Fig. 6 is in embodiment 1, the hysteresis curve of the cobalt prepared by hydrolysis under room temperature-nickel bimetal hydroxide nanometer complexes, as can be seen from the figure hysteresis curve is narrower, saturation magnetization is 5.34emu/g, coercivity is 80Oe, therefore preparation cobalt-the nickel bimetal hydroxide nanometer complexes is a kind of ferrimagnet.
Embodiment 2: catalysis p-nitrophenol hydrogenation:
By the freshly prepd sodium borohydride solution of the p-nitrophenyl phenol solution of 0.1 milliliter of 0.004M, 2 ml distilled waters, 1 milliliter of 0.1M, be added to successively in quartz colorimetric utensil in order, the color of solution is immediately by the light yellow glassy yellow that becomes, simultaneously absworption peak by 317 nanometer red shifts to 400 nanometers left and right, add subsequently the cobalt of 1 milligram of preparation-nickel bimetal hydroxide nanometer complexes, with ultraviolet specrophotometer, between the 200-500 nanometer, every 1 minute, test once, until the peak of 400 nanometers left and right does not significantly change.
Adopt Shimadzu UV-1750 ultraviolet specrophotometer to test the catalysis p-nitrophenol hydrogenation character of sample.
The ultraviolet-ray visible absorbing curve that Fig. 7, Fig. 8 are the at room temperature catalysis p-nitrophenol hydrogenation of the present embodiment product, as seen from Figure 7, after adding the sodium borohydride solution that 1 milliliter of freshly prepd concentration is 0.1M, the position of absworption peak by 317 nanometer red shifts to 400 about nanometers.As seen from Figure 8, along with the reduction gradually of 400 nanometers absorption peak strength, 300 nanometer left and right have occurred that a new absworption peak and intensity raise gradually, and this absworption peak is the absworption peak of the para-aminophenol ion of reduction generation.After adding 1 milligram of cobalt-nickel bimetal hydroxide nanometer complexes, only needing 6 minutes just can be complete by the p-nitrophenol solution catalyzing of 0.1 milliliter of 0.004M.

Claims (2)

1. the preparation method of cobalt-nickel bimetal hydroxide nanometer complexes, content comprises: weighing 0.146 gram cabaltous nitrate hexahydrate and 0.200 gram polyvinylpyrrolidone (PVP) ultrasonic dissolution are in 40 ml distilled waters, then be transferred to three-neck flask, open the rotating speed agitating solution that electric blender arranges 1000 rev/mins.Under stirring condition, drip 40 milliliters of new configuration with syringe pump containing 0.750 gram sodium borohydride aqueous solution, within 15 minutes, drip.Subsequently, with syringe pump, drip 40 milliliters containing the 0.119 gram Nickel dichloride hexahydrate aqueous solution, within 15 minutes, drip.After all reagent adds, solution continues stirring reaction one hour, after reaction finishes, by solution centrifugal, collects the black solid product, with distilled water and ethanol, respectively washs three times, 60 degrees centigrade of oven dry, obtains sample.
2. the application of the cobalt that as claimed in claim 1 prepared by method-nickel bimetal hydroxide nanometer complexes to catalyzing organic hydrogenation, be characterised in that described organic matter is p-nitrophenol.
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Cited By (9)

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CN103979615A (en) * 2014-04-28 2014-08-13 河南大学 Boron doped with alpha-Ni(OH)2, preparation method and application thereof
CN105334251A (en) * 2015-11-16 2016-02-17 安徽师范大学 Tremella-like Fe-Ni layered double hydroxides, oxygen evolution electrode as well as preparation methods and applications thereof
CN106449136A (en) * 2016-09-05 2017-02-22 郑州大学 Alpha-nickel hydroxide cobalt electrode material and preparation method and application thereof
CN107128981A (en) * 2017-06-12 2017-09-05 南京晓庄学院 Ni M O H are nanocrystalline and its controllable type synthetic method and the application in ultracapacitor is prepared
CN107915262A (en) * 2017-11-08 2018-04-17 华东师范大学 A kind of preparation method of two-dimensional ultrathin hydroxide
CN109133200A (en) * 2018-08-31 2019-01-04 哈尔滨理工大学 A kind of preparation of flower-shape Ni-Co hydrotalcite electrode material
CN109679386A (en) * 2019-01-11 2019-04-26 安徽大学 A kind of normal temperature cured type transparent inorganic water resistant coating and preparation method thereof
CN110882702A (en) * 2019-12-16 2020-03-17 生态环境部环境规划院 Preparation method and application of catalytic material based on magnetic layered double hydroxide
CN111961217A (en) * 2020-08-26 2020-11-20 合肥工业大学 Preparation method and application of amorphous metal oxide induced NiCo-BTC nanosheet

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103979615A (en) * 2014-04-28 2014-08-13 河南大学 Boron doped with alpha-Ni(OH)2, preparation method and application thereof
CN103979615B (en) * 2014-04-28 2016-04-13 河南大学 Boron doped alpha-Ni (OH) 2and preparation method thereof, purposes
CN105334251A (en) * 2015-11-16 2016-02-17 安徽师范大学 Tremella-like Fe-Ni layered double hydroxides, oxygen evolution electrode as well as preparation methods and applications thereof
CN105334251B (en) * 2015-11-16 2018-05-25 安徽师范大学 The Fe-Ni double-metal hydroxides of class tremelliform analyse oxygen electrode and its preparation method and application
CN106449136A (en) * 2016-09-05 2017-02-22 郑州大学 Alpha-nickel hydroxide cobalt electrode material and preparation method and application thereof
CN106449136B (en) * 2016-09-05 2019-04-05 郑州大学 Alpha-nickel hydroxide cobalt electrode material and the preparation method and application thereof
CN107128981A (en) * 2017-06-12 2017-09-05 南京晓庄学院 Ni M O H are nanocrystalline and its controllable type synthetic method and the application in ultracapacitor is prepared
CN107128981B (en) * 2017-06-12 2018-07-13 南京晓庄学院 Ni-M-O-H is nanocrystalline and its controllable type synthetic method and the application in preparing ultracapacitor
CN107915262A (en) * 2017-11-08 2018-04-17 华东师范大学 A kind of preparation method of two-dimensional ultrathin hydroxide
CN109133200A (en) * 2018-08-31 2019-01-04 哈尔滨理工大学 A kind of preparation of flower-shape Ni-Co hydrotalcite electrode material
CN109679386A (en) * 2019-01-11 2019-04-26 安徽大学 A kind of normal temperature cured type transparent inorganic water resistant coating and preparation method thereof
CN110882702A (en) * 2019-12-16 2020-03-17 生态环境部环境规划院 Preparation method and application of catalytic material based on magnetic layered double hydroxide
CN111961217A (en) * 2020-08-26 2020-11-20 合肥工业大学 Preparation method and application of amorphous metal oxide induced NiCo-BTC nanosheet
CN111961217B (en) * 2020-08-26 2022-04-22 合肥工业大学 Preparation method and application of amorphous metal oxide induced NiCo-BTC nanosheet

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