CN112404447A - Preparation method and application of metallic nickel - Google Patents
Preparation method and application of metallic nickel Download PDFInfo
- Publication number
- CN112404447A CN112404447A CN202011289993.0A CN202011289993A CN112404447A CN 112404447 A CN112404447 A CN 112404447A CN 202011289993 A CN202011289993 A CN 202011289993A CN 112404447 A CN112404447 A CN 112404447A
- Authority
- CN
- China
- Prior art keywords
- product
- intermediate product
- nickel
- reaction
- metallic nickel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The application provides a preparation method and application of metallic nickel, wherein the preparation method comprises the following steps: mixing nickel salt and carbazole, indole, quinoline or isoquinoline according to a molar ratio of 5:1-1:2, adding a solvent, and uniformly stirring and mixing to obtain a mixed solution; placing the mixed solution into a heating container for constant-temperature heating reaction at 90-150 ℃ for 24-96 h to obtain a reaction product; taking out the reaction product, cooling to normal temperature, filtering the precipitate, washing and drying to obtain an intermediate product; and (3) placing the intermediate product at the temperature of 100-170 ℃, introducing hydrogen with certain pressure to carry out constant-pressure reduction, and reacting for 8-12 h to obtain the product metallic nickel. The metallic nickel prepared by the scheme has high purity, simple preparation method and good effect in the aspect of hydrogen storage catalysis application.
Description
Technical Field
The application relates to the technical field of catalyst preparation, in particular to a preparation method and application of metallic nickel.
Background
Hydrogen energy is used as a green energy source and is an energy carrier and fuel with sustainable development potential. The hydrogen energy economy developed on the basis of hydrogen energy has the characteristics of zero emission and good economic and environmental benefits, and meets the development requirements of future energy policies of China. However, the use of hydrogen energy has long been greatly hindered by the lack of convenient and effective hydrogen storage materials and techniques.
In recent years, researchers have conducted extensive research around hydrogen storage materials, wherein the development of liquid hydrogen storage materials is mature and has a relatively complete industrial chain. However, the liquid hydrogen storage material can not be separated from the catalyst, and the hydrogen absorption and desorption process can be carried out only under the condition that the catalyst is used. In the prior art, the commonly used catalyst is a metal catalyst, such as platinum, ruthenium, nickel and the like, but the precious metals such as platinum, ruthenium and the like have high cost and are not suitable for large-scale popularization and application. Compared with the nickel, the nickel has higher cost performance and better application prospect. The purity of the metal catalyst directly influences the catalytic effect, and further influences the hydrogen storage effect of the hydrogen storage material, and in the preparation method of the metal nickel in the prior art, the metal nickel with higher purity is difficult to prepare, so that the wide application of the liquid hydrogen storage material is limited. Therefore, there is a need to develop a method for preparing high-purity metallic nickel.
Disclosure of Invention
The application provides a preparation method of metallic nickel and application thereof, which aims to solve the problem that no mature preparation method of high-purity metallic nickel exists at present.
In a first aspect, an embodiment of the present application provides a method for preparing metallic nickel, where the method includes:
mixing nickel salt and carbazole, indole, quinoline or isoquinoline according to a molar ratio of 5:1-1:2, adding a solvent, and uniformly stirring and mixing to obtain a mixed solution;
placing the mixed solution into a heating container for constant-temperature heating reaction at 90-150 ℃ for 24-96 h to obtain a reaction product;
taking out the reaction product, cooling to normal temperature, filtering the precipitate, washing and drying to obtain an intermediate product;
and (3) placing the intermediate product at the temperature of 100-170 ℃, introducing hydrogen with certain pressure to carry out constant-pressure reduction, and reacting for 8-12 h to obtain the product metallic nickel.
With reference to the first aspect, in one implementation manner, after obtaining the intermediate product, the preparation method further includes:
and (3) placing the intermediate product at the temperature of 250-300 ℃ for pretreatment for 20-30 min to obtain an activated product.
With reference to the first aspect, in one implementation manner, the intermediate product is activated by vacuum pumping at 250 ℃ for 30min by using a high-pressure gas adsorption tester to obtain an activated product.
In one implementation in combination with the first aspect, the nickel nitrate and carbazole are mixed in a molar ratio of 2:1, 1:2, or 5: 1.
In one implementation in combination with the first aspect, the nickel nitrate and the indole are mixed in a molar ratio of 2:1, 1:2, or 5: 1.
In one implementation in combination with the first aspect, the nickel nitrate is mixed with quinoline or isoquinoline in a molar ratio of 2:1, 1:2, or 5: 1.
With reference to the first aspect, in one implementation manner, the solvent is a mixed solution of ultrapure water and N-dimethylformamide.
With reference to the first aspect, in one implementation, the heating vessel is a metal reaction kettle or an oil bath.
With reference to the first aspect, in one implementation manner, the reaction temperature is 140 ℃ and the reaction time is 72 h.
In a second aspect, the application provides an application of metallic nickel, and the metallic nickel prepared by any one of the preparation methods in the first aspect is applied to hydrogen storage catalysis.
The application provides a preparation method and application of metallic nickel, wherein the preparation method comprises the following steps: mixing nickel salt and carbazole, indole, quinoline or isoquinoline according to a molar ratio of 5:1-1:2, adding a solvent, and uniformly stirring and mixing to obtain a mixed solution; placing the mixed solution into a heating container for constant-temperature heating reaction at 90-150 ℃ for 24-96 h to obtain a reaction product; taking out the reaction product, cooling to normal temperature, filtering the precipitate, washing and drying to obtain an intermediate product; and (3) placing the intermediate product at the temperature of 100-170 ℃, introducing hydrogen with certain pressure to carry out constant-pressure reduction, and reacting for 8-12 h to obtain the product metallic nickel. The metallic nickel prepared by the scheme has high purity, simple preparation method and good effect in the aspect of hydrogen storage catalysis application.
Drawings
In order to more clearly explain the technical solution of the present application, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious to those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic flow chart of a method for preparing metallic nickel provided by an embodiment of the present application;
FIG. 2 is an XRD characteristic spectrum of an intermediate product provided by an embodiment of the present application;
figure 3 is an XRD characteristic line of the final product provided in the examples of the present application.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present application more comprehensible, the present application is described in further detail with reference to the accompanying drawings and the detailed description.
The embodiment of the application provides a preparation method of metallic nickel and application thereof, which aim to solve the problem that no mature preparation method of high-purity metallic nickel exists at present.
The embodiment of the application discloses a preparation method of metallic nickel, and with reference to fig. 1, the preparation method comprises the following steps:
s1, mixing the nickel salt and carbazole, indole, quinoline or isoquinoline according to the molar ratio of 5:1-1:2, adding the solvent, and uniformly stirring and mixing to obtain a mixed solution.
In the step, firstly, nickel salt and carbazole, indole, quinoline or isoquinoline are taken according to a certain proportion (the molar ratio is 5:1-1:2), then a certain amount of solvent is taken, the amount of the solvent is determined according to the amount of the raw materials, and then the three are stirred and mixed uniformly to obtain a mixed solution.
Preferably, this step may include: mixing nickel nitrate and carbazole according to a molar ratio of 2:1, 1:2 or 5:1, adding a solvent, and uniformly stirring and mixing to obtain a mixed solution.
Or mixing nickel nitrate and indole according to the mol ratio of 2:1, 1:2 or 5:1, adding a solvent, and uniformly stirring and mixing to obtain a mixed solution.
Or mixing nickel nitrate and quinoline or isoquinoline according to the molar ratio of 2:1, 1:2 or 5:1, adding a solvent, and uniformly stirring and mixing to obtain a mixed solution.
Optionally, the solvent is ultrapure water or N-Dimethylformamide (DMF), or a mixture of ultrapure water and N-dimethylformamide.
S2, placing the mixed solution into a heating container to be heated and reacted at a constant temperature of 90-150 ℃ for 24-96 h to obtain a reaction product.
In the step, the constant temperature can be realized by adopting a constant temperature box, the temperature of the constant temperature box can be controlled to be 140 ℃, and the reaction time is set to be 72 h.
Optionally, the heating container is a metal reaction kettle or an oil bath kettle, and the lining of the metal reaction kettle is polytetrafluoroethylene.
In this step, the raw material and the solvent in step S1 are subjected to a sufficient reaction by a hydrothermal reaction to obtain a reaction product.
S3, taking out the reaction product, cooling to normal temperature, filtering the precipitate, washing and drying to obtain an intermediate product.
In the step, conventional technologies can be adopted for filtering, washing and drying, and a washing solvent, washing times and drying temperature are selected according to the characteristics of the reaction product, and the method is not particularly limited in the application.
The step is a process of processing a reaction product to obtain an intermediate product, wherein the intermediate product obtained in the step is Ni3(NO3)2(OH)4The intermediate product is characterized as shown in FIG. 2, FIG. 2 is the XRD characteristic line of the intermediate product, the abscissa is angle () and the ordinate is Intensity, and the material can be confirmed to be Ni by searching from the XRD characteristic spectrum library3(NO3)2(OH)4。
S4, placing the intermediate product at 100-170 ℃, introducing hydrogen with certain pressure to carry out constant pressure reduction, and reacting for 8-12 h to obtain the product metallic nickel.
In the step, the intermediate product obtained in the step S3 is subjected to hydrogenation reduction to obtain a final product, and the final product is characterized as shown in fig. 3, fig. 3 is an XRD characteristic spectrum line of the final product, and the XRD characteristic spectrum line is retrieved from an XRD characteristic spectrum library to show that the substance is metallic nickel, and the product has high purity and substantially no impurity peak.
In the application, the intermediate product is crystallized and precipitated, and the metallic nickel powder with smaller granularity can be prepared by controlling the reaction conditions.
The preparation method is simple, the preparation cost is low, the preparation raw materials are simple, and no additional by-product is generated in the preparation process, so that the purity of the metal nickel is higher, and the preparation method can be widely used.
Accordingly, the present application provides a method for preparing metallic nickel, wherein the method for preparing comprises: mixing nickel salt and carbazole, indole, quinoline or isoquinoline according to a molar ratio of 5:1-1:2, adding a solvent, and uniformly stirring and mixing to obtain a mixed solution; placing the mixed solution into a heating container for constant-temperature heating reaction at 90-150 ℃ for 24-96 h to obtain a reaction product; taking out the reaction product, cooling to normal temperature, filtering the precipitate, washing and drying to obtain an intermediate product; and (3) placing the intermediate product at the temperature of 100-170 ℃, introducing hydrogen with certain pressure to carry out constant-pressure reduction, and reacting for 8-12 h to obtain the product metallic nickel. The metallic nickel prepared by the scheme has high purity, simple preparation method and good effect in the aspect of hydrogen storage catalysis application.
Optionally, in the above preparation process, after obtaining the intermediate product, i.e., after step S3, the preparation method further includes:
and (3) placing the intermediate product at the temperature of 250-300 ℃ for pretreatment for 20-30 min to obtain an activated product.
Before hydrogenation reduction, the activation aims to facilitate the next hydrogenation reduction, so that the reduction is more thorough, the purity of the obtained metallic nickel is further improved, meanwhile, the hydrogenation reduction time can be shortened, the product metallic nickel can be obtained after reaction for 2-3 h, and the cost is saved. Specifically, the intermediate product is vacuumized and activated for 30min at 250 ℃ by using a high-pressure gas adsorption tester to obtain an activated product.
After the activation step is added, in the step S4, the activated product is placed at 100-170 ℃, hydrogen with certain pressure is introduced for constant pressure reduction, and the product metallic nickel can be obtained after reaction for 8-12 h.
Other steps are similar to those described above, and the details of the preparation process can be found in the above.
Based on the preparation method disclosed above, the application also discloses the application of the metallic nickel prepared by the preparation method in hydrogen storage catalysis.
In order to make the specific process of preparing metallic nickel more clear by the above preparation method, the following examples of the specific preparation process and comparative examples are further illustrated.
Comparative example
2.4608g of nickel nitrate was taken and reacted with 20mL of DMF +30mL of ultrapure water as a solvent by a solvothermal (hydrothermal) method in a metal reaction kettle at 140 ℃ for 72 hours in a constant temperature drying oven, and no intermediate product was produced.
Example 1
Taking nickel nitrate and carbazole according to a molar ratio of 2:1, taking a mixture of 20mL of DMF and 30mL of ultrapure water as a solvent, reacting for 72 hours in a constant-temperature drying oven at 130 ℃ by using a metal reaction kettle by a solvent thermal (hydrothermal) method, carrying out suction filtration, washing and drying to obtain an intermediate product, and carrying out XRD characterization on the intermediate product, wherein a characteristic spectrum is shown in figure 2. And (3) vacuumizing and activating the intermediate product for 30min at 250 ℃ by using a high-pressure gas adsorption tester, filling hydrogen into the activated intermediate product, reacting for 3h at 150 ℃, and performing XRD characterization on the final product, wherein the characteristic spectrum is shown in figure 3.
Example 2
Taking nickel nitrate and carbazole according to a molar ratio of 1:2, taking 20mL of DMF +30mL of ultrapure water as a solvent, reacting for 72 hours in a constant-temperature drying oven at 140 ℃ by using a metal reaction kettle by adopting a solvothermal (hydrothermal) method, carrying out suction filtration, washing and drying to obtain an intermediate product, and carrying out XRD (X-ray diffraction) characterization on the intermediate product, wherein a characteristic spectrum is shown in figure 2. And (3) vacuumizing and activating the intermediate product for 30min at 250 ℃ by using a high-pressure gas adsorption tester, filling hydrogen into the activated intermediate product, reacting for 3h at 150 ℃, and performing XRD characterization on the final product, wherein the characteristic spectrum is shown in figure 3.
Example 3
Taking nickel nitrate and carbazole according to a molar ratio of 5:1, taking 20mL of DMF +30mL of ultrapure water as a solvent, adding the raw materials into a round-bottom flask, reacting for 36 hours in an oil bath kettle at 140 ℃, filtering, washing and drying to obtain an intermediate product, and carrying out XRD characterization on the intermediate product, wherein a characteristic spectrum is shown in figure 2. And (3) carrying out hydrogen reduction on the intermediate product by using a high-pressure gas adsorption instrument, filling hydrogen, reacting for 9 hours at 120 ℃, and carrying out XRD characterization on the final product, wherein the characteristic spectrum is shown in figure 3.
Example 4
Taking nickel nitrate and indole according to a molar ratio of 2:1, taking 20mL of DMF +30mL of ultrapure water as a solvent, reacting for 72 hours in a constant-temperature drying oven at 130 ℃ by using a metal reaction kettle by adopting a solvothermal (hydrothermal) method, carrying out suction filtration, washing and drying to obtain an intermediate product, and carrying out XRD (X-ray diffraction) characterization on the intermediate product, wherein a characteristic spectrum is shown in figure 2. And (3) vacuumizing and activating the intermediate product for 30min at 250 ℃ by using a high-pressure gas adsorption tester, filling hydrogen into the activated intermediate product, reacting for 3h at 150 ℃, and performing XRD characterization on the final product, wherein the characteristic spectrum is shown in figure 3.
Example 5
Taking nickel nitrate and indole according to a molar ratio of 1:2, taking a mixture of 20mL of DMF and 30mL of ultrapure water as a solvent, reacting for 72 hours in a constant-temperature drying oven at 140 ℃ by using a metal reaction kettle by a solvothermal (hydrothermal) method, carrying out suction filtration, washing and drying to obtain an intermediate product, and carrying out XRD (X-ray diffraction) characterization on the intermediate product, wherein a characteristic spectrum is shown in figure 2. And (3) vacuumizing and activating the intermediate product for 30min at 250 ℃ by using a high-pressure gas adsorption tester, filling hydrogen into the activated intermediate product, reacting for 3h at 150 ℃, and performing XRD characterization on the final product, wherein the characteristic spectrum is shown in figure 3.
Example 6
Taking nickel nitrate and indole according to a molar ratio of 5:1, taking 20mL of DMF +30mL of ultrapure water as a solvent, adding the raw materials into a round-bottom flask, reacting for 36 hours in an oil bath kettle at 140 ℃, filtering, washing and drying to obtain an intermediate product, and carrying out XRD characterization on the intermediate product, wherein a characteristic spectrum is shown in figure 2. And (3) carrying out hydrogen reduction on the intermediate product by using a high-pressure gas adsorption instrument, filling hydrogen, reacting for 9 hours at 120 ℃, and carrying out XRD characterization on the final product, wherein the characteristic spectrum is shown in figure 3.
Example 7
Taking nickel nitrate and quinoline according to the mol ratio of 2:1, taking deionized water as a solvent, reacting for 72 hours in a constant-temperature drying box at 140 ℃ by using a metal reaction kettle by adopting a solvothermal (hydrothermal) method, carrying out suction filtration, washing and drying to obtain an intermediate product, and carrying out XRD (X-ray diffraction) characterization on the intermediate product, wherein the characteristic spectrum is shown in figure 2. And (3) vacuumizing and activating the intermediate product for 30min at 250 ℃ by using a high-pressure gas adsorption tester, filling hydrogen into the activated intermediate product, reacting for 3h at 150 ℃, and performing XRD characterization on the final product, wherein the characteristic spectrum is shown in figure 3.
Example 8
Taking nickel nitrate and quinoline according to the molar ratio of 1:2, taking deionized water as a solvent, reacting for 72 hours in a constant-temperature drying box at 140 ℃ by using a metal reaction kettle by adopting a solvothermal (hydrothermal) method, carrying out suction filtration, washing and drying to obtain an intermediate product, and carrying out XRD (X-ray diffraction) characterization on the intermediate product, wherein the characteristic spectrum is shown in figure 2. And (3) vacuumizing and activating the intermediate product for 30min at 250 ℃ by using a high-pressure gas adsorption tester, filling hydrogen into the activated intermediate product, reacting for 3h at 150 ℃, and performing XRD characterization on the final product, wherein the characteristic spectrum is shown in figure 3.
Example 9
Taking nickel nitrate and quinoline according to the molar ratio of 5:1, taking deionized water as a solvent, adding the raw materials into a round bottom flask, reacting for 36 hours at 140 ℃ in an oil bath kettle, carrying out suction filtration, washing and drying to obtain an intermediate product, and carrying out XRD characterization on the intermediate product, wherein the characteristic spectrum is shown in figure 2. And (3) vacuumizing and activating the intermediate product for 30min at 200 ℃ by using a high-pressure gas adsorption tester, filling hydrogen into the activated intermediate product, reacting for 2h at 120 ℃, and performing XRD characterization on the final product, wherein the characteristic spectrum is shown in figure 3.
Example 10
Taking nickel nitrate and isoquinoline according to the molar ratio of 2:1, taking deionized water as a solvent, adding the raw materials into a round bottom flask, reacting for 72 hours in an oil bath kettle at the temperature of 140 ℃, carrying out suction filtration, washing and drying to obtain an intermediate product, and carrying out XRD characterization on the intermediate product, wherein the characteristic spectrum is shown in figure 2. And (3) vacuumizing and activating the intermediate product for 30min at 200 ℃ by using a high-pressure gas adsorption tester, filling hydrogen into the activated intermediate product, reacting for 2h at 120 ℃, and performing XRD characterization on the final product, wherein the characteristic spectrum is shown in figure 3.
Example 11
Taking nickel nitrate and quinoline according to the mol ratio of 2:1, taking deionized water as a solvent, adding the raw materials into a round bottom flask, reacting for 72 hours in an oil bath kettle at the temperature of 140 ℃, carrying out suction filtration, washing and drying to obtain an intermediate product, and carrying out XRD characterization on the intermediate product, wherein the characteristic spectrum is shown in figure 2. Filling hydrogen into the intermediate product in a high-pressure gas adsorption tester, reacting for 8h at 120 ℃, and carrying out XRD characterization on the final product, wherein the characteristic spectrum is shown in figure 3.
The present application has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to limit the application. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the presently disclosed embodiments and implementations thereof without departing from the spirit and scope of the present disclosure, and these fall within the scope of the present disclosure. The protection scope of this application is subject to the appended claims.
Claims (10)
1. A preparation method of metallic nickel is characterized by comprising the following steps:
mixing nickel salt and carbazole, indole, quinoline or isoquinoline according to a molar ratio of 5:1-1:2, adding a solvent, and uniformly stirring and mixing to obtain a mixed solution;
placing the mixed solution into a heating container for constant-temperature heating reaction at 90-150 ℃ for 24-96 h to obtain a reaction product;
taking out the reaction product, cooling to normal temperature, filtering the precipitate, washing and drying to obtain an intermediate product;
and (3) placing the intermediate product at the temperature of 100-170 ℃, introducing hydrogen with certain pressure to carry out constant-pressure reduction, and reacting for 8-12 h to obtain the product metallic nickel.
2. The method of claim 1, wherein after obtaining the intermediate product, the method further comprises:
and (3) placing the intermediate product at the temperature of 250-300 ℃ for pretreatment for 20-30 min to obtain an activated product.
3. The method according to claim 2, wherein the intermediate product is activated by vacuum-pumping with a high-pressure gas adsorption tester at 250 ℃ for 30min to obtain an activated product.
4. The method according to claim 1, wherein the nickel nitrate and the carbazole are mixed in a molar ratio of 2:1, 1:2, or 5: 1.
5. The method according to claim 1, wherein the nickel nitrate and the indole are mixed in a molar ratio of 2:1, 1:2 or 5: 1.
6. The process according to claim 1, wherein the nickel nitrate is mixed with quinoline or isoquinoline in a molar ratio of 2:1, 1:2 or 5: 1.
7. The production method according to claim 1, wherein the solvent is a mixed solution of ultrapure water and N-dimethylformamide.
8. The production method according to claim 1, wherein the heating vessel is a metal reaction vessel or an oil bath.
9. The method according to claim 1, wherein the reaction temperature is 140 ℃ and the reaction time is 72 hours.
10. Use of metallic nickel, characterized in that the metallic nickel prepared by the method of any one of claims 1 to 9 is used in hydrogen storage catalysis.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011289993.0A CN112404447B (en) | 2020-11-18 | 2020-11-18 | Preparation method and application of metallic nickel |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011289993.0A CN112404447B (en) | 2020-11-18 | 2020-11-18 | Preparation method and application of metallic nickel |
Publications (2)
Publication Number | Publication Date |
---|---|
CN112404447A true CN112404447A (en) | 2021-02-26 |
CN112404447B CN112404447B (en) | 2023-07-07 |
Family
ID=74831563
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202011289993.0A Active CN112404447B (en) | 2020-11-18 | 2020-11-18 | Preparation method and application of metallic nickel |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112404447B (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113773350A (en) * | 2021-07-16 | 2021-12-10 | 云南电网有限责任公司电力科学研究院 | Metal complex hydrogen storage material and preparation method thereof |
CN115532266A (en) * | 2022-09-27 | 2022-12-30 | 西安交通大学 | Ni-Cu/AC catalyst for preparing gas fuel by hydrothermal conversion of indole and derivatives thereof and preparation method thereof |
Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1345118A (en) * | 1971-06-14 | 1974-01-30 | Sherritt Gordon Mines Ltd | Production of nickel powder from basic nickel carbonate |
US4541861A (en) * | 1984-09-13 | 1985-09-17 | The Royal Institution For The Advancement Of Learning (Mcgill University) | Process for the production of cobalt, nickel and copper powders from chelating extractants |
RU2043301C1 (en) * | 1991-06-25 | 1995-09-10 | Аксенов Николай Никитович | Method for production of copper, zinc, nickel and cobalt basic carbonates and oxides |
US5584908A (en) * | 1994-11-14 | 1996-12-17 | Sherritt Inc. | Micron-sized nickel metal powder and a process for the preparation thereof |
CN101428348A (en) * | 2008-07-29 | 2009-05-13 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
CN107088660A (en) * | 2017-07-03 | 2017-08-25 | 张成亮 | A kind of preparation method of ultra-fine cobalt nickel powder |
CN107098404A (en) * | 2017-06-12 | 2017-08-29 | 太原理工大学 | Alkali formula nickel nitrate powder and preparation method and application with high rate capability |
CN110523970A (en) * | 2018-05-24 | 2019-12-03 | 中国石油化工股份有限公司 | A kind of carbon-coating nickel nano-particle and preparation method thereof |
CN110756820A (en) * | 2018-07-25 | 2020-02-07 | 荆门市格林美新材料有限公司 | Preparation method of single-sphere-like nickel powder |
CN110961652A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of lanthanum-doped superfine nickel powder |
CN110961647A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of molybdenum-doped superfine nickel powder |
CN111266602A (en) * | 2018-12-04 | 2020-06-12 | 荆门市格林美新材料有限公司 | Preparation method of superfine cobalt-nickel powder for hard alloy |
-
2020
- 2020-11-18 CN CN202011289993.0A patent/CN112404447B/en active Active
Patent Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1345118A (en) * | 1971-06-14 | 1974-01-30 | Sherritt Gordon Mines Ltd | Production of nickel powder from basic nickel carbonate |
US4541861A (en) * | 1984-09-13 | 1985-09-17 | The Royal Institution For The Advancement Of Learning (Mcgill University) | Process for the production of cobalt, nickel and copper powders from chelating extractants |
RU2043301C1 (en) * | 1991-06-25 | 1995-09-10 | Аксенов Николай Никитович | Method for production of copper, zinc, nickel and cobalt basic carbonates and oxides |
US5584908A (en) * | 1994-11-14 | 1996-12-17 | Sherritt Inc. | Micron-sized nickel metal powder and a process for the preparation thereof |
CN101428348A (en) * | 2008-07-29 | 2009-05-13 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
CN107098404A (en) * | 2017-06-12 | 2017-08-29 | 太原理工大学 | Alkali formula nickel nitrate powder and preparation method and application with high rate capability |
CN107088660A (en) * | 2017-07-03 | 2017-08-25 | 张成亮 | A kind of preparation method of ultra-fine cobalt nickel powder |
CN110523970A (en) * | 2018-05-24 | 2019-12-03 | 中国石油化工股份有限公司 | A kind of carbon-coating nickel nano-particle and preparation method thereof |
CN110756820A (en) * | 2018-07-25 | 2020-02-07 | 荆门市格林美新材料有限公司 | Preparation method of single-sphere-like nickel powder |
CN110961652A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of lanthanum-doped superfine nickel powder |
CN110961647A (en) * | 2018-09-28 | 2020-04-07 | 荆门市格林美新材料有限公司 | Preparation method of molybdenum-doped superfine nickel powder |
CN111266602A (en) * | 2018-12-04 | 2020-06-12 | 荆门市格林美新材料有限公司 | Preparation method of superfine cobalt-nickel powder for hard alloy |
Non-Patent Citations (1)
Title |
---|
李铁晶等: "配位沉淀-直接还原法制备球形超细镍粉", 《矿冶工程》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113773350A (en) * | 2021-07-16 | 2021-12-10 | 云南电网有限责任公司电力科学研究院 | Metal complex hydrogen storage material and preparation method thereof |
CN115532266A (en) * | 2022-09-27 | 2022-12-30 | 西安交通大学 | Ni-Cu/AC catalyst for preparing gas fuel by hydrothermal conversion of indole and derivatives thereof and preparation method thereof |
CN115532266B (en) * | 2022-09-27 | 2023-11-21 | 西安交通大学 | Ni-Cu/AC catalyst for preparing gas fuel by hydrothermally converting indole and derivative thereof and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
CN112404447B (en) | 2023-07-07 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110756203B (en) | Ni2P/Mn0.3Cd0.7S photocatalytic water splitting composite catalyst and preparation method and application thereof | |
CN109289855B (en) | Methanol catalyst for synthesis gas and preparation method thereof | |
CN112404447B (en) | Preparation method and application of metallic nickel | |
CN109705168B (en) | Binuclear nickel coordination compound and preparation method and application thereof | |
CN115591582B (en) | MOF-303/g-C 3 N 4 Heterojunction material and preparation method and application thereof | |
CN113441160B (en) | Nickel hydroxide/titanium carbide photo-thermal catalytic material and preparation method and application thereof | |
CN109772394B (en) | Phosphorus-doped carbon/cuprous oxide composite catalyst and preparation method and application thereof | |
CN113731441B (en) | Cobalt-reduced graphene oxide Co/rGO catalyst and preparation method and application thereof | |
CN115155600A (en) | Catalyst for synthesizing methanol and preparation method and application thereof | |
CN103769211B (en) | A kind of preparation method of the hybrid inorganic-organic materials supported ruthenium catalyst for the synthesis of L-aminopropanol | |
CN113603648B (en) | Cobalt complex and preparation method and application thereof | |
CN114425375B (en) | Ni 12 P 5 TpPa-1-COF photocatalyst, preparation method thereof and application thereof in photocatalytic water splitting | |
CN115960040A (en) | Cyano-containing modified cobalt tetrabipyridine complex as well as preparation method and application thereof | |
CN114182293B (en) | Preparation method of Ru-based catalyst with controllable particle size and application of Ru-based catalyst in' renewable energy electrolysis hydrogen production-ammonia synthesis | |
WO2021172107A1 (en) | Metal-loaded article containing typical element oxide, catalyst for ammonia synthesis and method for synthesizing ammonia | |
CN110813375B (en) | Preparation method and application of ultralong hollow chain spherical carbon nitride photocatalytic material | |
CN112547107A (en) | alpha-Fe2O3/Ni@2D g-C3N4Process for preparing catalyst | |
CN112358509A (en) | Metal organic complex solid hydrogen storage material and preparation method thereof | |
CN110317233A (en) | Metallic nickel and Metallic Manganese Complex and the preparation method and application thereof | |
CN115197280B (en) | Metal cobalt complex with photocatalytic carbon dioxide reduction activity and preparation method and application thereof | |
CN116393175B (en) | Carbon dioxide reduction catalyst, preparation method and application | |
CN115872897B (en) | Schiff base cobalt complex, preparation method and application thereof | |
CN115920887A (en) | In-situ grown copper-containing photocatalyst, preparation method and application thereof in reduction synthesis of ammonia by nitrate | |
CN115806573A (en) | Mononuclear cobalt complex, and preparation method and application thereof | |
CN116874390A (en) | Mononuclear cobalt complex based on Salen ligand, preparation method and application thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |