CN106379949B - A kind of preparation method of nickel tungstate nano wire - Google Patents
A kind of preparation method of nickel tungstate nano wire Download PDFInfo
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- CN106379949B CN106379949B CN201610990505.6A CN201610990505A CN106379949B CN 106379949 B CN106379949 B CN 106379949B CN 201610990505 A CN201610990505 A CN 201610990505A CN 106379949 B CN106379949 B CN 106379949B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of preparation method of nickel tungstate nano wire, have main steps that the deionized water solution for first preparing sodium tungstate, nickel sulfate, sodium carboxymethylcellulose respectively, then nickel sulfate and carboxymethylcellulose sodium solution are mixed, stirring 30 minutes, this mixed solution is mixed with sodium tungstate solution again, then after the mixture is carried out ultrasonically treated 30 minutes, finally carry out hydro-thermal process and obtain nickel tungstate nano wire.The preparation method for the nickel tungstate nano wire that the present invention is provided, has the advantages that simple to operate, morphology controllable, with low cost, it is easy to accomplish industrialized production；Prepared nickel tungstate nano wire has one-dimentional structure, and draw ratio is high, and specific surface area is big, has purposes widely in fields such as catalyst, optical fiber, capacitor, quick wet stock, laser, conducting material, detector, sensors.
Description
Technical field
The present invention relates to technical field of inorganic non-metal material preparation, specifically a kind of preparation side of nickel tungstate nano wire
Method.
Background technology
Nickel tungstate is a kind of very important functional material, in catalyst, optical fiber, capacitor, quick wet stock, laser
The fields such as device, conducting material, detector, sensor all have purposes widely.And the performance of nano material depends on receiving
The factors such as meter Jing Ti pattern and size, thus the nickel tungstate nanocrystal with special appearance is prepared, ground in theoretical foundation
Study carefully and practical application aspect all has very important significance.
Wherein, monodimension nanometer material with higher draw ratio and specific surface area because often showing especially excellent thing
Physicochemical performance, is one of study hotspot in recent years.The common method for preparing nano wire at present is template.Template is usual
Need by alumina formwork, with cost height, complex operation, and can only obtain multicrystal nano-wire, it is impossible to obtain monocrystalline and receive
The shortcomings of rice noodles.
In view of drawbacks described above, the invention provides a kind of preparation method of nickel tungstate nano wire, with technical process it is simple,
With low cost the advantages of, and the pattern of nickel tungstate nanocrystal can be efficiently controlled.Prepared nickel tungstate of the invention is received
Rice noodles, with one-dimentional structure, draw ratio is high, larger specific surface area, catalyst, optical fiber, capacitor, quick wet stock,
The fields such as laser, conducting material, detector, sensor, which have, to be more widely applied.
The content of the invention
It is an object of the invention to provide a kind of preparation method of nickel tungstate nano wire, technical process is simple, with low cost, energy
The pattern of enough effectively control nickel tungstate nanocrystals, prepared nickel tungstate nano wire has one-dimentional structure, and draw ratio is high, larger
Specific surface area, in catalyst, optical fiber, capacitor, quick wet stock, laser, conducting material, detector, sensor etc.
Field, which has, to be more widely applied.
The object of the invention to solve the technical problems is realized using following technical scheme.
According to a kind of preparation method of nickel tungstate nano wire proposed by the present invention, comprise the following steps：
1) nickel sulfate is dissolved in deionized water, forms nickel sulfate solution；
2) sodium carboxymethylcellulose is dissolved in deionized water, forms sodium carboxymethyl cellulose solution；
3) by step 1) made from nickel sulfate solution and step 2) made from sodium carboxymethyl cellulose solution mix,
Then stir 30 minutes, obtain the mixed solution of nickel sulfate and sodium carboxymethylcellulose；
4) sodium tungstate is dissolved in deionized water, forms wolframic acid sodium water solution；
5) by step 3) made from sodium carboxymethylcellulose and nickel sulfate mixed solution and step 4) made from sodium tungstate
The aqueous solution is mixed, then will be equipped with the mixture container be put into ultrasonic wave carry out it is ultrasonically treated；
6) by step 5) carry out it is ultrasonically treated after mixture be added in reactor inner bag, with distilled water adjust reactor
Reaction mass volume in inner bag reaches the 70%-90% of reactor inner bag volume；
7) by step 6) it is placed in equipped with the reactor inner bag of reaction mass in reactor, seal, carry out hydro-thermal process, then
Allow reactor to naturally cool to room temperature, unload after kettle, with distilled water cyclic washing reaction product, after filtering, drying, obtain nickel tungstate
Nano wire.
The object of the invention to solve the technical problems can be also applied to the following technical measures to achieve further.
A kind of preparation method of foregoing nickel tungstate nano wire, wherein, nickel sulfate in step (1) described nickel sulfate solution
Concentration be 0.04-1.2mol/L.
A kind of preparation method of foregoing nickel tungstate nano wire, wherein, step (2) described sodium carboxymethyl cellulose solution
In sodium carboxymethylcellulose concentration be 0.01-0.02mol/L.
A kind of preparation method of foregoing nickel tungstate nano wire, wherein, sodium tungstate in step (4) the wolframic acid sodium water solution
Concentration be 0.04-1.2mol/L.
The preparation method of foregoing nickel tungstate nano wire a kind of, wherein, sodium tungstate and nickel sulfate rub when step (5) is mixed
You are than being 1:1.
A kind of preparation method of foregoing nickel tungstate nano wire, wherein, ultrasonic power is 200- when step (5) is ultrasonically treated
1000W, ultrasonic time is 30-60 minutes.
A kind of preparation method of foregoing nickel tungstate nano wire, wherein, the method for step (7) described hydro-thermal process is：
5-12 hours are incubated at 180-220 DEG C.
A kind of preparation method of foregoing nickel tungstate nano wire, wherein, described sodium carboxymethylcellulose, sodium tungstate, sulphur
It is pure that the purity of sour nickel is not less than chemistry.
The key problem in technology point of the present invention is：First sodium carboxymethyl cellulose solution must mutually be mixed with nickel sulfate solution
Close, it is necessary to by the mixed solution of sodium tungstate solution and sodium carboxymethylcellulose and nickel sulfate mix carry out it is ultrasonically treated, it is no
It then cannot get nickel tungstate nano wire.
The present invention has clear advantage and beneficial effect compared with prior art, by above-mentioned technical proposal, the present invention
A kind of preparation method of nickel tungstate nano wire can reach suitable technological progress and practicality, and with the extensive profit in industry
With value, it at least has following advantages：
(1) preparation method of nickel tungstate nano wire that the present invention is provided, with simple to operate, morphology controllable, with low cost
The advantages of, it is easy to industrialized production.
(2) method of the invention has prepared good crystallinity, purity height, the nickel tungstate nano wire with one-dimentional structure, its
Purity is more than 99%, and a diameter of 10-50nm of nano wire, length is 1-3um, and draw ratio is more than 100, and specific surface area is
90.3m2/g.The nickel tungstate nano wire has one-dimentional structure, and draw ratio is high, and specific surface area is big, in catalyst, optical fiber, electricity
The fields such as container, quick wet stock, laser, conducting material, detector, sensor, which have, to be more widely applied.
In summary, a kind of preparation method of nickel tungstate nano wire of the invention technically has significant progress, and has
Obvious good effect, is really a new and innovative, progressive, practical new design.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, and in order to allow the above and other objects, features and advantages of the present invention can
Become apparent, below especially exemplified by preferred embodiment, and coordinate accompanying drawing, describe in detail as follows.
Brief description of the drawings
Fig. 1 is the XRD spectrum for the nickel tungstate nano wire that the present invention is synthesized；
Fig. 2 is transmission electron microscope (TEM) photo for the nickel tungstate nano wire that the present invention is synthesized.
Embodiment
Further to illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below in conjunction with
Accompanying drawing and preferred embodiment further illustrate the present invention.
Embodiment 1
1) nickel sulfate is dissolved in deionized water, the concentration for forming nickel sulfate in nickel sulfate solution, regulation solution is
0.3mol/L；
2) sodium carboxymethylcellulose is dissolved in deionized water, formed in sodium carboxymethyl cellulose solution, regulation solution
The concentration of sodium carboxymethylcellulose is 0.01mol/L；
3) by step 1) made from nickel sulfate solution and step 2) made from sodium carboxymethyl cellulose solution mix,
Then stir 30 minutes；
4) sodium tungstate is dissolved in deionized water, the concentration for forming sodium tungstate in wolframic acid sodium water solution, regulation solution is
0.3mol/L；
5) by step 3) made from sodium carboxymethylcellulose and nickel sulfate mixed solution and step 4) made from sodium tungstate water
Solution mix (wherein the mol ratio of sodium tungstate and nickel sulfate be 1:1) container that, then will be equipped with mixture is put into ultrasonic wave
Middle progress is ultrasonically treated, and ultrasonic power is 500W, and ultrasonic time is 40 minutes.
6) by step 5) carry out it is ultrasonically treated after mixture be added in reactor inner bag, with distilled water adjust reactor
Reaction mass volume in inner bag reaches the 70% of reactor inner bag volume；
7) by step 6) it is placed in equipped with the reactor inner bag of reaction mass in reactor, seal, 12 are incubated at 180 DEG C small
Shi Jinhang hydro-thermal process, then allows reactor to naturally cool to room temperature, unloads after kettle, with distilled water cyclic washing reaction product, mistake
After filter, drying, nickel tungstate nano wire is obtained, the diameter of nickel tungstate nano wire is about 10-30nm, and length is about 1.5-2um, its
XRD spectrum is shown in Fig. 1；Transmission electron microscope picture is shown in Fig. 2.
Embodiment 2
1) nickel sulfate is dissolved in deionized water, the concentration for forming nickel sulfate in nickel sulfate solution, regulation solution is
0.65mol/L；
2) sodium carboxymethylcellulose is dissolved in deionized water, formed in sodium carboxymethyl cellulose solution, regulation solution
The concentration of sodium carboxymethylcellulose is 0.015mol/L；
3) by step 1) made from nickel sulfate solution and step 2) made from sodium carboxymethyl cellulose solution mix,
Then stir 30 minutes；
4) sodium tungstate is dissolved in deionized water, the concentration for forming sodium tungstate in wolframic acid sodium water solution, regulation solution is
0.65mol/L；
5) by step 3) made from sodium carboxymethylcellulose and nickel sulfate mixed solution and step 4) made from sodium tungstate water
Solution mix (wherein the mol ratio of sodium tungstate and nickel sulfate be 1:1) container that, then will be equipped with the mixture is put into ultrasound
Carry out ultrasonically treated in ripple, ultrasonic power is 800W, and ultrasonic time is 50 minutes.
6) by step 5) carry out it is ultrasonically treated after mixture be added in reactor inner bag, with distilled water adjust reactor
Reaction mass volume in inner bag reaches the 80% of reactor inner bag volume；
7) by step 6) it is placed in equipped with the reactor inner bag of reaction mass in reactor, seal, 8 are incubated at 200 DEG C small
Shi Jinhang hydro-thermal process, then allows reactor to naturally cool to room temperature, unloads after kettle, with distilled water cyclic washing reaction product, mistake
After filter, drying, nickel tungstate nano wire is obtained.
Embodiment 3
1) nickel sulfate is dissolved in deionized water, the concentration for forming nickel sulfate in nickel sulfate solution, regulation solution is
1.1mol/L；
2) sodium carboxymethylcellulose is dissolved in deionized water, formed in sodium carboxymethyl cellulose solution, regulation solution
The concentration of sodium carboxymethylcellulose is 0.02mol/L；
3) by step 1) made from nickel sulfate solution and step 2) made from sodium carboxymethyl cellulose solution mix,
Then stir 30 minutes；
4) sodium tungstate is dissolved in deionized water, the concentration for forming sodium tungstate in wolframic acid sodium water solution, regulation solution is
1.1mol/L；
5) by step 3) made from sodium carboxymethylcellulose and nickel sulfate mixed solution and step 4) made from sodium tungstate water
Solution mix (wherein the mol ratio of sodium tungstate and nickel sulfate be 1:1) container that, then will be equipped with the mixture is put into ultrasound
Carry out ultrasonically treated in ripple, ultrasonic power is 1000W, and ultrasonic time is 60 minutes.
6) by step 5) carry out it is ultrasonically treated after mixture be added in reactor inner bag, with distilled water adjust reactor
Reaction mass volume in inner bag reaches the 90% of reactor inner bag volume；
7) by step 6) it is placed in equipped with the reactor inner bag of reaction mass in reactor, seal, 6 are incubated at 220 DEG C small
Shi Jinhang hydro-thermal process, then allows reactor to naturally cool to room temperature, unloads after kettle, with distilled water cyclic washing reaction product, mistake
After filter, drying, nickel tungstate nano wire is obtained.
It is pure that above-mentioned raw materials sodium carboxymethylcellulose, sodium tungstate, the purity of nickel sulfate are not less than chemistry.
The above described is only a preferred embodiment of the present invention, any formal limitation not is made to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any to be familiar with this professional technology people
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit according to the present invention
Any simple modification, equivalent variations and the modification made to above example, in the range of still falling within technical solution of the present invention.
Claims (5)
1. a kind of preparation method of nickel tungstate nano wire, it is characterised in that comprise the following steps：
1) nickel sulfate is dissolved in deionized water, forms nickel sulfate solution；
2) sodium carboxymethylcellulose is dissolved in deionized water, forms sodium carboxymethyl cellulose solution；
3) by step 1) made from nickel sulfate solution and step 2) made from sodium carboxymethyl cellulose solution mix, then
Stirring 30 minutes, obtains the mixed solution of nickel sulfate and sodium carboxymethylcellulose；
4) sodium tungstate is dissolved in deionized water, forms wolframic acid sodium water solution；
5) by step 3) made from sodium carboxymethylcellulose and nickel sulfate mixed solution and step 4) made from sodium tungstate it is water-soluble
Liquid phase is mixed, and the mol ratio of sodium tungstate and nickel sulfate is 1 during mixing:1, the container that then will be equipped with the mixture is put into ultrasonic wave
Middle progress is ultrasonically treated；Ultrasonically treated power is 200-1000W, and ultrasonic time is 30-60 minutes；
6) by step 5) carry out it is ultrasonically treated after mixture be added in reactor inner bag, with distilled water adjust reactor inner bag
In reaction mass volume reach the 70%-90% of reactor inner bag volume；
7) by step 6) it is placed in equipped with the reactor inner bag of reaction mass in reactor, seal, carry out hydro-thermal process, described water
Heat-treating methods are：5-12 hours are incubated at 180-220 DEG C；Then allow reactor to naturally cool to room temperature, unload after kettle, use
Distilled water cyclic washing reaction product, after filtering, drying, obtains nickel tungstate nano wire.
2. the preparation method of nickel tungstate nano wire according to claim 1, it is characterised in that step (1) the nickel sulfate water
The concentration of nickel sulfate is 0.04-1.2mol/L in solution.
3. the preparation method of nickel tungstate nano wire according to claim 1, it is characterised in that step (2) carboxymethyl is fine
The concentration of sodium carboxymethylcellulose in the plain sodium water solution of dimension is 0.01-0.02mol/L.
4. the preparation method of nickel tungstate nano wire according to claim 1, it is characterised in that step (4) the sodium tungstate water
The concentration of sodium tungstate is 0.04-1.2mol/L in solution.
5. the preparation method of nickel tungstate nano wire according to claim 1, it is characterised in that described carboxymethyl cellulose
It is pure that sodium, sodium tungstate, the purity of nickel sulfate are not less than chemistry.
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| CN107572604B (en) * | 2017-10-31 | 2021-04-02 | 南阳理工学院 | Preparation method of nickel tungstate nanorod supercapacitor material |
| CN111285411B (en) * | 2020-02-25 | 2022-08-12 | 杭州电子科技大学 | Preparation method of binary metal oxide nano material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5874056A (en) * | 1994-06-03 | 1999-02-23 | H.C Starck Gmbh & Co. Kg | Metal tungstates and method of preparing them and their use |
| CN102583587A (en) * | 2012-03-02 | 2012-07-18 | 河北联合大学 | Preparation of nickel tungstate nanometer disks with uniform diameter |
| CN102718262A (en) * | 2012-03-02 | 2012-10-10 | 河北联合大学 | Preparation of nanowire assembled calcium tungstate spherical structure |
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2016
- 2016-11-10 CN CN201610990505.6A patent/CN106379949B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5874056A (en) * | 1994-06-03 | 1999-02-23 | H.C Starck Gmbh & Co. Kg | Metal tungstates and method of preparing them and their use |
| CN102583587A (en) * | 2012-03-02 | 2012-07-18 | 河北联合大学 | Preparation of nickel tungstate nanometer disks with uniform diameter |
| CN102718262A (en) * | 2012-03-02 | 2012-10-10 | 河北联合大学 | Preparation of nanowire assembled calcium tungstate spherical structure |
Non-Patent Citations (1)
| Title |
|---|
| 王朝峰.NiWO4纳米粒子的合成、表征和加氢脱硫性能.《石油学报（石油加工）》.2013,331-335页. * |
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