CN107235909A - A kind of preparation method for the cobalt-based material for accumulating nanometer chip architecture - Google Patents

A kind of preparation method for the cobalt-based material for accumulating nanometer chip architecture Download PDF

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Publication number
CN107235909A
CN107235909A CN201710456596.XA CN201710456596A CN107235909A CN 107235909 A CN107235909 A CN 107235909A CN 201710456596 A CN201710456596 A CN 201710456596A CN 107235909 A CN107235909 A CN 107235909A
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cobalt
solution
preparation
chip architecture
based material
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CN201710456596.XA
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庞欢
肖潇
李欣冉
郭笑天
王建达
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Yangzhou University
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Yangzhou University
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
    • C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
    • C07D233/56—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms
    • C07D233/58—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring nitrogen atoms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Abstract

A kind of preparation method for the cobalt-based material for accumulating nanometer chip architecture, belongs to the preparing technical field of nano material, forms solution A by cobalt salt and transition metal salt mixed dissolution in methyl alcohol；Organic ligand is dissolved in methanol, organic ligand solution B is formed；Solution A and solution B are blended under ultrasound condition and reacted, zeolite imidazole class framework material 67 is obtained, then carry out hydro-thermal reaction is remixed with solution A, is then cleaned with methanol, the cobalt-based material of nanometer chip architecture must be accumulated.The present invention is simple to operate, and reaction is easily controlled, reproducible, pollution-free, and security is good, and the ratio of each metal salt in final obtained material is different, can prepare the different metal alloy particle of pattern.

Description

A kind of preparation method for the cobalt-based material for accumulating nanometer chip architecture
Technical field
The invention belongs to the preparing technical field of nano material, and in particular to the system of the cobalt-based material of accumulation nanometer chip architecture Preparation Method.
Background technology
Magnetic material is important functional material, as a kind of typical magnetic metal material, with each to different of uniqueness Property magnetic, to Magnetic Memory device, Magnetic Sensor, catalyst etc. application have important application value.
Two dimension（2D）Ultrathin nanometer piece is due to its unique structure, electronic transmission performance and physique, it has also become wide A series of general generally acknowledged energy source use materials.Ultrathin nanometer piece can not only make substantial amounts of surface-active site and large area with The intimate contact of electrolyte and electrode quick interface electric charge transfer provides a very high specific surface area, while also making more The high activity site of exposed inner atom is recombinated by surface.
Metal-organic framework material（MOF）, a kind of new porous part being made up of metal ion and cluster organic matter Material, has been widely studied.Various characterizing methods show that excellent bone framework and good pore structure fit MOF materials For ultracapacitor, sensor is adsorbed, in terms of drug delivery.Compared to other ligand materials it is high because high surface area Porosity, low-density, controlled architecture, adjustable aperture, MOFs materials are considered as most promising material in following nm regime One of.The size of the hole of MOFs material precursors can be tuned by changing organic ligand, and maximum diameter of hole is received for 9.8 Rice.
Two-dimentional MOF nanometer sheets show many peculiar properties for being different from conventional blocks MOF materials.Such as, theirs is super Flaky texture is conducive to the transmission of electronics, and then is conducive to improving the performance of electric energy storage device.Different from the work of bulk material Property site it is main inside MOF duct, two-dimentional MOF nanometer sheets can expose substantial amounts of avtive spot in sheet surfaces, be conducive to Contact of the substrate molecule with avtive spot, and then MOF is improved in catalysis or the performance of sensory field.Therefore, design synthesis two dimension The MOF materials of laminated structure are a critically important research directions, can not only improve the performance of MOF materials, can also be expanded New application field.
The content of the invention
The need for above prior art and market, the present invention provides a kind of cobalt-based material for accumulating nanometer chip architecture Preparation method.
The present invention comprises the following steps：
1）By cobalt salt and transition metal salt mixed dissolution in methyl alcohol, solution A is formed；
2）Organic ligand is dissolved in methanol, organic ligand solution B is formed；
3）After the solution A and solution B are mixed, reacted under ultrasound condition, obtain zeolite imidazole class framework material 67；
4）The zeolite imidazole class framework material 67 is remixed with solution A, water-filling is entered under 100~200 DEG C of constant temperature Thermal response；
5）After hydro-thermal reaction terminates, cleaned with methanol, the cobalt-based material of nanometer chip architecture must be accumulated.
6）In above-mentioned reactions steps 3）In, reacted under ultrasound condition, reaction composition granule more tinyization can be made, increased Plus contact area, make reaction carry out more quickly and thoroughly.
7）In above-mentioned reactions steps 4）In, 100~200 DEG C of hot conditions can increase the movement velocity of molecule, either Still kinetically all accelerate reaction speed in thermodynamics, make reaction carry out more quickly and thoroughly.
The present invention utilizes the nontoxic a series of high-quality cobalt-based nano material of Material synthesis, and reasonable in design, operation Simply, reaction is easily controlled, reproducible, pollution-free, and security is good.Cobalt salt and transition of the present invention by using different proportion Metal salt is reacted, and the ratio of each metal salt in final obtained material is different, can prepare the different gold of pattern Belong to alloying pellet.
Compared with prior art, the present invention is prepared from by simple hydro-thermal method, the raw material of use are nontoxic, environmentally friendly, into This is low, and technique is simple, it is easy to operational control, suitable for continuous large-scale production, preparation process environmental protection.
Further, cobalt salt of the present invention is Co (NO3)2•6H2O, in actual experiment, because nitrate anion is easily sloughed, It is more easy to obtain required product, therefore preferentially uses this several nickelate.
The transition metal salt is nickel salt, mantoquita, manganese salt or zinc salt.In actual experiment, because this several salt is inexpensive easily , relatively stablize, therefore preferentially use this several transition metal salt.
The organic ligand is 2-methylimidazole.2-methylimidazole is common organic ligand, inexpensive and be easy to get, therefore preferentially Using.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of intermediate product zeolite imidazole class framework material 67.
Fig. 2 is the stereoscan photograph of the obtained accumulation nanometer sheet of example 1.
Fig. 3 is the stereoscan photograph of the obtained accumulation nanometer sheet of example 2.
Fig. 4 is the stereoscan photograph of the obtained accumulation nanometer sheet of example 3.
Fig. 5 is the stereoscan photograph of the obtained accumulation nanometer sheet of example 4.
Embodiment
The present invention will be further described for example below, but not limited to this.
The pattern of packed structures nanometer sheet prepared by following embodiment passes through supra-55 type SEM （SEM）Photo is shown.
Embodiment 1：
（1）0.53g Co (NO are weighed respectively3)2•6H2O, 0.0174g Ni (NO3)2•6H2O, is dissolved in 15mL methanol solution In, obtain 15mL solution As.Wherein cobalt nickel mol ratio is 30: 1.
（2）The 2-methylimidazole for weighing 0.616g is dissolved in 15mL methanol solutions, forms 15mL solution B.
（3）Solution A is added drop-wise to rapidly step（2）In the solution B of acquirement, and ultrasound 15min obtains intermediate product zeolite Imidazoles framework material 67（Abbreviation ZIF-67）.
（4）By step（3）In the centrifugation of intermediate product zeolite imidazole class framework material 67 come out and be dissolved in 15mL methanol In solution, the methanol solution of 15mL zeolite imidazole class framework material 67 is obtained.
（5）By step（4）The methanol solution of obtained zeolite imidazole class framework material 67 is mixed with 15mL solution As, and Hydro-thermal reaction 1h is carried out under 100~120 DEG C of environmental conditions.
After the completion of hydro-thermal reaction, repeatedly washed with methanol, obtain product.
Embodiment 2：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step be the same as Example 1, except that cobalt nickel mol ratio is 10∶1。
Embodiment 3：
The preparation method of the cobalt-based material of nanometer chip architecture, step be the same as Example 1 are accumulated, except that cobalt nickel mol ratio is 5 ∶1。
Embodiment 4：
The preparation method of the cobalt-based material of nanometer chip architecture, step be the same as Example 1 are accumulated, except that cobalt nickel mol ratio is 1 ∶1。
Fig. 1 show the stereoscan photograph of intermediate product zeolite imidazole class framework material 67, obtains as can be seen from Figure Intermediate product it is uniform in size, in perfect hexahedron structure.
It is 30: 1 that Fig. 2, which show cobalt nickel mol ratio made from example 1, the stereoscan photograph of nanometer sheet is accumulated, from figure It can be seen that sample is the chondritic that nanometer sheet is accumulated, nanometer sheet thickness is uniform.
It is 10: 1 that Fig. 3, which show cobalt nickel mol ratio made from example 2, the stereoscan photograph of nanometer sheet is accumulated, from figure It can be seen that sample is the chondritic that nanometer sheet is accumulated, with the increase of nickel salt mole, nanometer sheet thickness increase.
It is 5: 1 that Fig. 4, which show cobalt nickel mol ratio made from example 3, accumulates the stereoscan photograph of nanometer sheet, can from figure To find out the chondritic that sample is accumulated as nanometer sheet, nanometer sheet thickness continues to increase.
It is 1: 1 that Fig. 5, which show cobalt nickel mol ratio made from example 4, accumulates the stereoscan photograph of nanometer sheet, can from figure To find out the near-spherical structure that sample is accumulated as nanometer sheet, intensive chondritic starts to weaken.
Embodiment 5：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step class be the same as Example 1, except that Ni (NO3)2• 6H2O is changed to Cu (NO3)2•3H2O。
Embodiment 6：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step class be the same as Example 2, except that Ni (NO3)2• 6H2O is changed to Cu (NO3)2•3H2O。
Embodiment 7：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step class be the same as Example 3, except that Ni (NO3)2• 6H2O is changed to Cu (NO3)2•3H2O。
Embodiment 8：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step class be the same as Example 4, except that Ni (NO3)2• 6H2O is changed to Cu (NO3)2•3H2O。
Embodiment 9：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step class be the same as Example 1, except that Ni (NO3)2• 6H2O is changed to MnSO4•H2O。
Embodiment 10：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step class be the same as Example 2, except that Ni (NO3)2• 6H2O is changed to MnSO4•H2O。
Embodiment 11：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step class be the same as Example 3, except that Ni (NO3)2• 6H2O is changed to MnSO4•H2O。
Embodiment 12：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step be the same as Example 4, except that Ni (NO3)2•6H2O It is changed to MnSO4•H2O。
Embodiment 13：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step be the same as Example 1, except that Ni (NO3)2•6H2O It is changed to C4H6O4Zn•2H2O。
Embodiment 14：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step be the same as Example 2, except that Ni (NO3)2•6H2O It is changed to C4H6O4Zn•2H2O。
Embodiment 15：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step be the same as Example 3, except that Ni (NO3)2•6H2O It is changed to C4H6O4Zn•2H2O。
Embodiment 16：
Accumulate the preparation method of the cobalt-based material of nanometer chip architecture, step be the same as Example 4, except that Ni (NO3)2•6H2O It is changed to C4H6O4Zn•2H2O。
The product of the acquirement of above example 5 to 16 is shown by supra-55 type SEM, its result class Be the same as Example 1 to 4.

Claims (4)

1. a kind of preparation method for the cobalt-based material for accumulating nanometer chip architecture, it is characterised in that comprise the following steps：
1）By cobalt salt and transition metal salt mixed dissolution in methyl alcohol, solution A is formed；
2）Organic ligand is dissolved in methanol, organic ligand solution B is formed；
3）After the solution A and solution B are mixed, reacted under ultrasound condition, obtain zeolite imidazole class framework material 67；
4）The zeolite imidazole class framework material 67 is remixed with solution A, water-filling is entered under 100~200 DEG C of constant temperature Thermal response；
5）After hydro-thermal reaction terminates, cleaned with methanol, the cobalt-based material of nanometer chip architecture must be accumulated.
2. preparation method according to claim 1, it is characterised in that the cobalt salt is Co (NO3)2•6H2O。
3. preparation method according to claim 1, it is characterised in that the transition metal salt be nickel salt, mantoquita, manganese salt or Zinc salt.
4. preparation method according to claim 1, it is characterised in that the organic ligand is 2-methylimidazole.
CN201710456596.XA 2017-06-16 2017-06-16 A kind of preparation method for the cobalt-based material for accumulating nanometer chip architecture Pending CN107235909A (en)

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Cited By (9)

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Publication number Priority date Publication date Assignee Title
CN107778494A (en) * 2017-11-02 2018-03-09 扬州大学 A kind of preparation method of nickel cobalt metal-organic framework materials
CN108033492A (en) * 2017-12-19 2018-05-15 扬州大学 The CoWO of amorphous4The preparation method of cage-shaped nano material and its application in electro-catalysis
CN108346522A (en) * 2018-03-28 2018-07-31 安徽师范大学 A kind of cobaltosic oxide hierarchical structure nano-array material, preparation method and applications
CN110280269A (en) * 2019-07-19 2019-09-27 曲阜师范大学 A kind of the cobalt-based petal-shaped composite material and preparation method and application of silver nano-grain load
CN108126703B (en) * 2018-01-11 2020-08-04 扬州大学 Embroidered spherical CuZnOXPreparation method of nano material and application of nano material in electrocatalysis
CN111995760A (en) * 2020-07-17 2020-11-27 扬州大学 Cobalt-metal organic framework nanosheet and preparation method and application thereof
CN112058268A (en) * 2020-09-07 2020-12-11 北京理工大学 Preparation method of zeolite imidazolyl metal organic framework nanosheet for oxygen reduction reaction
CN113968594A (en) * 2021-10-21 2022-01-25 南京理工大学 Method for preparing Ni-Co bimetal compound by one-step aqueous solvent method
CN114522712A (en) * 2022-02-22 2022-05-24 嘉兴学院 Amphiphilic CoP/g-C for degrading micro-plastic and synergistically producing hydrogen3N4Material and method for producing same

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107778494A (en) * 2017-11-02 2018-03-09 扬州大学 A kind of preparation method of nickel cobalt metal-organic framework materials
CN108033492A (en) * 2017-12-19 2018-05-15 扬州大学 The CoWO of amorphous4The preparation method of cage-shaped nano material and its application in electro-catalysis
CN108126703B (en) * 2018-01-11 2020-08-04 扬州大学 Embroidered spherical CuZnOXPreparation method of nano material and application of nano material in electrocatalysis
CN108346522A (en) * 2018-03-28 2018-07-31 安徽师范大学 A kind of cobaltosic oxide hierarchical structure nano-array material, preparation method and applications
CN108346522B (en) * 2018-03-28 2020-01-10 安徽师范大学 Cobaltosic oxide hierarchical structure nano array material, preparation method and application thereof
CN110280269A (en) * 2019-07-19 2019-09-27 曲阜师范大学 A kind of the cobalt-based petal-shaped composite material and preparation method and application of silver nano-grain load
CN111995760A (en) * 2020-07-17 2020-11-27 扬州大学 Cobalt-metal organic framework nanosheet and preparation method and application thereof
CN112058268A (en) * 2020-09-07 2020-12-11 北京理工大学 Preparation method of zeolite imidazolyl metal organic framework nanosheet for oxygen reduction reaction
CN113968594A (en) * 2021-10-21 2022-01-25 南京理工大学 Method for preparing Ni-Co bimetal compound by one-step aqueous solvent method
CN113968594B (en) * 2021-10-21 2024-02-13 南京理工大学 Method for preparing Ni-Co bimetallic compound by one-step water solvent method
CN114522712A (en) * 2022-02-22 2022-05-24 嘉兴学院 Amphiphilic CoP/g-C for degrading micro-plastic and synergistically producing hydrogen3N4Material and method for producing same
CN114522712B (en) * 2022-02-22 2023-12-01 嘉兴学院 Amphiphilic CoP/g-C for synergistic hydrogen production of degraded microplastic 3 N 4 Material and preparation method thereof

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