CN102502891B - Preparation method for nickel molybdate nanorod material - Google Patents
Preparation method for nickel molybdate nanorod material Download PDFInfo
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- CN102502891B CN102502891B CN 201110347426 CN201110347426A CN102502891B CN 102502891 B CN102502891 B CN 102502891B CN 201110347426 CN201110347426 CN 201110347426 CN 201110347426 A CN201110347426 A CN 201110347426A CN 102502891 B CN102502891 B CN 102502891B
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Abstract
The invention relates to a preparation method for nickel molybdate nanorod material, comprising the following steps of: using ammonium molybdate and nickel chloride as reactants, using sodium dodecyl benzene sulfonate as a structure-directing agent, and utilizing microwave radiation heating means in a synthesis system for nanometre material. The nickel molybdate nanorod material has the advantages of being regular in shape and uniform in size, and the single nanorod is only 10 to 25 nanometres in diameter; the bundle-shaped structure assembled by a plurality of nanorods is 100 to 200 nanometres in diameter and 1.3 to 1.7 microns in length. In the preparation system, the structure-directing agent sodium dodecyl benzene sulfonate is good in hydrophilcity and convenient for post-cleaning andpost-treatment for product, and is thus good for obtaining high-purity target product. The synthesis method provides technical support for system research for the structure-activity relationship between the microscopic structure and the performance of the nickel molybdate nanorod material, and accumulates a certain practical experience for promotion for the low-cost scale production and the general application of material simultaneously.
Description
[technical field]: the invention belongs to field of inorganic nano-material preparation, particularly relate to a kind of preparation method of nickel molybdate nano-bar material.
[background technology]: in recent years, adding structure directing agent in the chemical reaction system provides the important channel for the nano material that designs synthetic specific morphology, and has caused the extensive interest of the many researchers of materials chemistry.For example, Sodium dodecylbenzene sulfonate can the nano material initial stage during nucleation selectively induced nuclei towards specific axis to oriented growth, thereby have influence on the final microscopic appearance of material.
Nickel molybdate, as the important component part in the metal molybdate, because having remarkable catalytic activity and lubricating property, be used as organism hydrogenating desulfurization/nitrogen catalyzer, oil dope, solid lubricant etc., thereby represent bright application prospect in fields such as petrochemical complex, machinofacture.Present stage, though the nickel molybdate nano material has already been used technology such as high temperature solid-state method, coprecipitation method, sol-gel method, hydrothermal method, combustion synthesis method, but synthetic pattern mostly is form of spherical particles, bulk or sheet (as: B.Moreno, E.Chinarro, M.T.Colomer, J.R.Jurado, J.Phys.Chem.C, 2010,114,4251; K.Eda, Y.Ohshiro, N.Nagai, N.Sotani, M.S.Whittingham, J.Solid State Chem., 2009,182,55.).And less about other preparation report of nickel molybdate with special appearance, and there are deficiencies such as complicated operation, productive rate are low in the partial synthesis technology.At the key issue that exists in the above-mentioned preparation process, patent of the present invention provides a kind of preparation method of nickel molybdate nano-bar material, and it is structure directing agent with the Sodium dodecylbenzene sulfonate, and the applied microwave radiation method successfully synthesizes the nickel molybdate one dimension Nano structure; This synthetic method provides technical support for the structure activity relationship between the systematic study nickel molybdate nano material micro-structure and property, has also accumulated certain practical experience for low-coat scale production and the widespread usage that promotes material simultaneously.
[summary of the invention]: the summary of the invention of this patent is to provide a kind of preparation method of nickel molybdate nano-bar material, it adopts microwave irradiation technology, and in reaction system, on purpose add the Sodium dodecylbenzene sulfonate to optimize the material habit, come the efficient oriented growth in order of induced material, thereby prepare the one dimension nickel molybdate nano-bar material of pattern novelty, thereby establish good research basis for performance optimization.
[technical scheme of the present invention]: patent of the present invention relates to a kind of preparation method of nickel molybdate nano-bar material, it is reactant with ammonium molybdate and nickelous chloride, Sodium dodecylbenzene sulfonate is as structure directing agent, and adopt the carry out microwave radiation heating means in the nano material synthetic system, comprise the steps:
The first, the Sodium dodecylbenzene sulfonate of weighing certain mass joins in the distilled water, and adds nickelous chloride crystal NiCl
26H
2O is stirred well to solid and dissolves fully;
The second, with the ammonium molybdate (NH of certain mass
4)
6Mo
7O
244H
2O joins in the distilled water, the ammonium molybdate solution of preparation certain concentration;
Three, two kinds of solution that step 1, two is disposed fully mix, and are transferred to then in the normal pressure microwave radiation reaction unit and act on 30 minutes;
Four, the gained flocks places 70～80 ℃ of freeze-day with constant temperature after 24 hours after centrifugal, distilled water cleans 5～7 times, absolute ethanol washing 1～3 time again, just obtains consisting of NiMoO
4The nickel molybdate nano-bar material.
The volumetric molar concentration of described nickelous chloride is that the volumetric molar concentration of 0.300mol/L, Sodium dodecylbenzene sulfonate is that the volumetric molar concentration of 0.030 mol, ammonium molybdate is 0.043mol/L.
The pattern of described nickel molybdate nano-bar material is regular, the uniform characteristics of size, and its single nanometer rod diameter only is 10～25 nanometers; The diameter that many nanometer rod are assembled into fascircular texture is that 100～200 nanometers, length are 1.3～1.7 microns.
[advantage of the present invention and effect]: patent disclosure of the present invention a kind of method that adopts the synthetic nickel molybdate nanometer rod of microwave irradiation, it has the following advantages and beneficial effect: 1, raw material sources are extensive, cheap and easy to get; 2, structure directing agent Sodium dodecylbenzene sulfonate possess hydrophilic property is good, be convenient to product later stage clean, obtain high-purity target product thereby be beneficial to, by the auxiliary microwave irradiation energy of Sodium dodecylbenzene sulfonate controlledly synthesis nickel molybdate nanometer rod, finally realized the effective control to appearance of nano material; 3, He Cheng nickel molybdate nanometer rod is expected to as high activated catalyst and favorable industrial lubricant because of the microtexture characteristics.
[description of drawings]:
Fig. 1 is low power scanning electronic microscope (SEM) figure of nickel molybdate nanometer rod
Fig. 2 is the high power SEM figure of nickel molybdate nanometer rod
[embodiment]:
Embodiment: the preparation method of nickel molybdate nanometer rod and structural characterization
The Sodium dodecylbenzene sulfonate of weighing certain mass joins in the distilled water, and adds the nickelous chloride crystal, is stirred well to solid and dissolves fully, and with the nickel chloride solution of preparation 0.300mol/L, the volumetric molar concentration of Sodium dodecylbenzene sulfonate is 0.030 mol; The volumetric molar concentration that other prepares ammonium molybdate solution is 0.043mol/L; Then above-mentioned two kinds of solution are mixed and are transferred in the microwave radiation reaction unit and act on 30 minutes; At last with the gained flocks after centrifugal, distilled water cleans 6 times, absolute ethanol washing 2 times, after 24 hours, just obtain the nickel molybdate nano-bar material at 70 ℃ of freeze-day with constant temperature again, it consists of NiMoO
4(Fig. 1) result shows that the nickel molybdate material is the club shaped structure of size homogeneous by this sample low power SEM test, and its length is 1.3～1.7 microns; By further observing as can be known than the SEM of high magnification figure (Fig. 2): the diameter of forming the nanometer rod of bar-shaped pattern only is 10～25 nanometers, and many nanometer rod are assembled into the fascircular texture of reunion, and its diameter is 100～200 nanometers.
Claims (1)
1. the preparation method of a nickel molybdate nano-bar material, it is reactant with ammonium molybdate and nickelous chloride, Sodium dodecylbenzene sulfonate is as structure directing agent, and adopts the carry out microwave radiation heating means in the nano material synthetic system, comprises the steps:
The first, the Sodium dodecylbenzene sulfonate of weighing certain mass joins in the distilled water, and adds nickelous chloride crystal NiCl
26H
2O is stirred well to solid and dissolves fully, and the volumetric molar concentration that makes nickelous chloride is that the volumetric molar concentration of 0.300mol/L, Sodium dodecylbenzene sulfonate is 0.030 mol;
The second, with the ammonium molybdate (NH of certain mass
4)
6Mo
7O
244H
2O joins in the distilled water, the ammonium molybdate solution of preparation certain concentration, and the volumetric molar concentration that makes ammonium molybdate is 0.043mol/L;
Three, two kinds of solution that step 1, two is disposed fully mix, and are transferred to then in the normal pressure microwave radiation reaction unit and act on 30 minutes;
Four, the gained flocks places 70～80 ℃ of freeze-day with constant temperature after 24 hours after centrifugal, distilled water cleans 5～7 times, absolute ethanol washing 1～3 time again, just obtains consisting of NiMoO
4The nickel molybdate nano-bar material; The pattern of described nickel molybdate nano-bar material is regular, size is even, and its single nanometer rod diameter only is 10～25 nanometers; The diameter that many nanometer rod are assembled into fascircular texture is that 100～200 nanometers, length are 1.3～1.7 microns.
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| CN103449537B (en) * | 2013-08-19 | 2015-08-26 | 长安大学 | A kind of preparation method of nickel molybdate powder material |
| CN105097300B (en) * | 2015-08-01 | 2018-02-16 | 东北电力大学 | A kind of NiMoO4/MoS2The preparation method of/NiS nano composite materials |
| CN106298261B (en) * | 2016-09-23 | 2018-05-25 | 安徽师范大学 | A kind of Co3O4@NiO@NiMoO4Heterogeneous nano array structure material, preparation method and applications |
| CN109423268B (en) * | 2017-09-04 | 2020-11-13 | 中国石油化工股份有限公司 | Underground modified viscosity reducer for thickened oil and preparation method thereof |
| CN107978460A (en) * | 2017-11-21 | 2018-05-01 | 信阳师范学院 | A kind of preparation method of electrode material for super capacitor multilayer petal-shaped nickel molybdate |
| CN109095515A (en) * | 2018-09-21 | 2018-12-28 | 新疆大学 | A kind of solid state reaction preparation β-NiMoO4The method of nanometer rods |
| CN111111680B (en) * | 2020-02-11 | 2022-11-18 | 湘潭大学 | Rodlike Ni-MoO 3-x Preparation method and application of catalyst |
| CN111807424B (en) * | 2020-07-23 | 2022-10-18 | 九江学院 | Granular NiMoO 4 Preparation method of electrode material |
| CN114349073B (en) * | 2021-12-30 | 2023-09-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of phosphorus-doped nickel molybdate negative electrode material |
| CN117577458A (en) * | 2023-12-06 | 2024-02-20 | 贵州大学 | NiMoO with nanorod-like structure 4 Is prepared through preparing process, its product and application |
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| CN102161509B (en) * | 2011-02-12 | 2013-04-03 | 河北联合大学 | Method for synthesizing metal molybdate micron/nano materials by adopting microwave radiation method |
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